美国药典USP31(921)翻译版(上)
美国药典USP31无菌检查
美国药典USP31无菌检查简介美国药典（United States Pharmacopeia，简称USP）是美国公认的医药行业标准组织，负责制定和发布有关医药品质量的标准和方法。
无菌检查是USP31中的一个重要章节，它主要用于评估药品、医疗器械和其他与患者直接接触的产品的无菌状态。
本文将介绍无菌检查的定义、方法和注意事项。
无菌检查的定义无菌检查是指对药品或医疗器械进行的一系列检验，以确定其是否存在可繁殖的微生物，从而判断其无菌性。
无菌状态是指在没有任何活体微生物存在的情况下。
对于注射剂、眼药水等需要直接进入体内的产品，无菌状态非常重要，以防止微生物感染和其他不良反应的发生。
无菌检查方法无菌检查的方法有多种，常用的方法包括：厌氧培养方法这种方法用于检测生长于缺氧条件下的微生物。
样品通常放置在厌氧培养基中，然后在恒温条件下培养，观察是否有菌落的形成。
高压蒸气灭菌法这种方法通过将样品暴露在高温高压的环境中，使用蒸汽来灭活可能存在的微生物。
灭菌后，用无菌培养基接种样品，并在一段时间后观察是否有菌落的形成。
过滤方法这种方法通过使用无菌过滤器来过滤样品，将可能存在的微生物滤除。
过滤后，将过滤膜接种在无菌培养基上，观察是否有菌落的形成。
光谱学方法这种方法通过使用紫外线、红外线等光谱技术来检测微生物的存在。
由于微生物具有特有的光谱特征，因此可以通过光谱仪器来进行无菌检查。
注意事项在进行无菌检查时，需要注意以下事项：检测设备的无菌性检测设备（培养皿、培养基等）在使用前应进行无菌处理，以避免外源性微生物的干扰。
常用的处理方法包括高温蒸馏、紫外线照射等。
样品的收集和处理在收集样品时，应注意避免样品与外界环境的接触，以防止样品被外源性微生物污染。
在处理样品时，应采取无菌操作，避免微生物的传播。
结果的解读在进行无菌检查后，需要对结果进行解读。
有菌落的形成通常表示样品存在微生物污染，是不符合无菌要求的。
无菌检查的结果应与相应的标准进行比较，以确定样品是否合格。
美国药典翻译凡例
凡例此颜色的为与USP28相比，新增的内容适用于美国药典的标准、实验、分析和其它规范说明。
凡例（后面提到的General Notices）和在通用章节中出现的general requirements以总则的形式提供美国药典中的标准、实验、分析和其它规范说明的解释与应用的基本指导，以消除整本书中与大量实例相关的那些要求的重复需要。
只要没有相反的特定说明，就应用凡例（General Notices）和通用章节（General Chapters）中的要求。
凡是不同于凡例（General Notices）和通用章节（General Chapters）时，将优先采用个论中的说法，并应特别指明其用法或内容。
为了强调这些例外的存在，在凡例（General Notices）和通用章节（General Chapters）的某些地方使用“除非另有规定”这样的措词。
在正文中，它（“除非另有规定”）应理解为标准、实验、分析或其它规范说明中与凡例（General Notices）和通用章节（General Chapters）中存在偏差的特殊规定，无论是否有例外的表述。
标题本出版物的标题，包括它的增补本，是美利坚合众国药典，第29版。
这个标题可被缩写为美国药典，第29版或USP 29。
美国药典，第29版取代了以前的所有版本。
凡是使用“USP”这个词的地方，没有更多的限制说明，在这本药典的法定期限内，仅指USP 29或相应的增补本。
相同的标题同样适用于包含这些内容的印刷版或电子版。
“OFFICIAL” AND “OFFICIAL ARTICLES”凡在药典或相应的参考中使用“official”,这个词，与“Pharmacopeial”，“USP”和“compendial”.是同义的。
若USP与法定名称相连，或在一物品标签上标上“USP”则表明USP收载了该个论并且该物品符合USP标准。
在标签上USP这个名称，既不可以也不能含生产商的标示的描写、签注或二者的合并，标示上有包含在USP正文中的信息材料，也不包含由USP保证这个物品符合USP标准。
美国药典-中英文对照(翻译资料)
美国药典－中英文对照译文美国药典中记载的辣椒碱资料辣椒碱（辣椒素）分子结构式：C18H27NO3，分子量：305.41，化学名：（反）－N－[（4－N－羟基－3－甲氧基苯基）－甲基]－8－甲基－6－壬烯基酰胺以干燥提取物计算，辣椒碱含辣椒二萜类化合物总量为标示量的90％－100%,其中辣椒素的含量达到50％以上，辣椒素和二氢辣椒素总量超过75％，其它辣椒素类化合物总量不足15％。
注意事项：小心处置辣椒碱，谨防吸入辣椒碱微粒，勿使身体接触辣椒碱。
包装贮藏：密封包装，置避光，阴凉处保存。
标示量：以辣椒二萜类化合物总百分含量表示。
美国药典参考标准：美国药典辣椒素标准规范，美国药典二氢辣椒素标准规范。
鉴别：配制1.0mg/ml辣椒碱甲醇溶液，配制符合美国药典标准的辣椒碱1.0mg/ml甲醇溶液作为对照液，分别点样于0.25mm厚硅胶、凝胶混合薄层板上，点样量为10礚，将薄层板放于乙醚－甲醇（19:1）展开剂中展开，待展开剂前沿至薄层板3/4处时将薄层板取出，晾干，用0.5% 2,6-二溴苯醌-氯化亚胺甲醇溶液喷雾显色，放于氨气中片刻，取出，鉴别色谱图：供试液主要斑点颜色（兰色）及R值与对照液主要斑点颜色（兰色）及R值一致。
熔点〈741〉: 57°－66°, 一般熔融起始温度至结束温度温差不超过5°。
干燥失重〈731〉: 置40°P2O5真空干燥器中干燥5小时，失重不超过1.0%。
灼烧残渣：≤1.0％。
辣椒素，二氢辣椒素及其它辣椒二萜类化合物含量测定：流动相：磷酸水溶液（l ：1000，V/V）：乙腈(600:400)混匀，0.5祄微孔滤膜滤过，脱气。
流动相视色谱行为可作适当调整。
辣椒素对照液：精密称取美国药典标准的辣椒碱适量溶于甲醇中，配制约0.1 mg/mL的辣椒甲醇溶液。
二氢辣椒素对照液：精密称取美国药典标准的辣椒碱适量溶于甲醇中，配制约0.025mg/mL的辣椒甲醇溶液。
美国药典USP31翻译版
Many Pharmacopeial articles either are hydrates or contain water in adsorbed form. As a result, the determination of the water content is important in demonstrating compliance with the Pharmacopeial standards. Generally one of the methods given below is called for in the individual monograph, depending upon the nature of the article. In rare cases, a choice is allowed between two methods. When the article contains water of hydration, the Method I (Titrimetric), the Method II (Azeotropic), or the Method III (Gravimetric) is employed, as directed in the individual monograph, and the requirement is given under the heading Water.很多药典物品要么是水合物，要么含有处于吸附状态的水。
因此，测定水分含量对于证实与药典标准的符合性是很重要的。
通常，在具体的各论中会根据该物品的性质，要求使用下面若干方法中的一个。
偶尔，会允许在2个方法中任选一个。
当该物品含有水合状态的水，按照具体各论中的规定，使用方法I（滴定测量法）、方法II（恒沸测量法）、或方法III（重量分析法），这个要求在标题水分项下给出。
美国药典e
146/Enzyme-Modified Fats/Monographs FCC VWater Determine as directed under Water Determination, Appendix IIB.Packaging and Storage Store in well-closed containers. Enzyme-Modified FatsDESCRIPTIONEnzyme-Modified Fats occur as light to medium tan liquids, pastes,or powders with a strong fatty acid odor and flavor. They are produced by enzyme lipolysis of fats obtained from milk,refined beef fat,or steam-rendered chicken fat,using suitable food-grade enzymes.Enzyme-modified milkfat may be prepared from milk,concentrated milk,dry whole milk, cream,concentrated cream(s),dry cream,butter,butter oil, dried butter,or anhydrous milkfat.For enzyme-modified milk-fat,optional dairy ingredients such as skim milk,concentrated skim milk,nonfat dry milk,buttermilk,concentrated butter-milk,dried buttermilk,liquid whey,concentrated whey,and dried whey may be used to adjust the concentration of the flavors.Fat emulsions are reacted with suitable food-grade enzymes under controlled conditions to increase the flavor components.Thermoprocessing is then used to destroy the enzyme activity and provide acceptable microbiological qual-ity.Suitable preservatives,emulsifiers,buffers,stabilizers, and antioxidants as well as sodium chloride may be added. The resulting product is concentrated or dried.Function Flavoring agent.REQUIREMENTSLabeling Indicate the Acid Value.Identification A sample has a very strong fatty acid odor. Acid Value Not less than98.0%and not more than102.0% of the labeled value.Lead Not more than1mg/kg.Loss on Drying Not more than4.0%for the dry product. Microbial Limits:Aerobic Plate Count Not more than10,000CFU per gram.Coliforms Not more than10CFU per gram. Salmonella Negative in25g.Staphylococcal Enterotoxins Negative in1g. Staphylococcus aureus Not more than100CFU per gram.Yeasts and Molds Not more than10CFU per gram.TESTSAcid Value Determine as directed in Method II under Acid Value,Appendix VII,using a5-g sample.Lead Determine as directed for Method II in the Atomic Absorption Spectrophotometric Graphite Furnace Method un-der Lead Limit Test,Appendix IIIB.Loss on Drying Determine as directed under Loss on Dry-ing,Appendix IIC,drying a sample at105°for48h. Microbial Limits(Note:Current methods for the following tests may be found online at</~ebam/ bam-toc.html>):Aerobic Plate CountColiformsSalmonellaStaphylococcal EnterotoxinsStaphylococcus aureusYeasts and MoldsPackaging and Storage Store in tight containers in a cool place.Enzyme PreparationsDESCRIPTIONEnzyme Preparations used in food processing are derived from animal,plant,or microbial sources(see Classification, below).They may consist of whole cells,parts of cells,or cell-free extracts of the source used,and they may contain one active component or,more commonly,a mixture of several,as well as food-grade diluents,preservatives,antioxidants,and other substances consistent with good manufacturing prac-tices.The individual preparations usually are named according to the substance to which they are applied,such as Protease or Amylase.Traditional names such as Malt,Pepsin,and Rennet also are used,however.The color of the preparations—which may be liquid,semi-liquid,or dry—may vary from virtually colorless to dark brown.The active components consist of the biologically active proteins,which are sometimes conjugated with metals, carbohydrates,and/or lipids.Known molecular weights of the active components range from approximately12,000to several hundred thousand.The activity of enzyme preparations is measured according to the reaction catalyzed by individual enzymes(see below) and is usually expressed in activity units per unit weight of the preparation.In commercial practice(but not for FoodFCC V Monographs/Enzyme Preparations/147Chemicals Codex purposes),the activity of the product is sometimes also given as the quantity of the preparation to be added to a given quantity of food to achieve the desired effect. Additional information relating to the nomenclature and the sources from which the active components are derived is provided under Enzyme Assays,Appendix V.Function Enzyme(see discussion under Classification, below).CLASSIFICATIONAnimal-Derived PreparationsCatalase,Bovine Liver Produced as partially purified liq-uid or powdered extracts from bovine liver.Major active principle:catalase.Typical application:used in the manufac-ture of certain cheeses.Chymotrypsin Obtained from purified extracts of bovine or porcine pancreatic tissue.Produced as white to tan,amorphous powders soluble in water,but practically insoluble in alcohol, in chloroform,and in ether.Major active principle:chymotryp-sin.Typical application:used in the hydrolysis of protein. Lipase,Animal Obtained from the edible forestomach tis-sue of calves,kids,or lambs;and from animal pancreatic tissue.Produced as purified edible tissue preparations or as aqueous extracts dispersible in water,but insoluble in alcohol. Major active principle:lipase.Typical applications:used in the manufacture of cheese and in the modification of lipids. Lysozyme Obtained from extracts of purified chicken egg whites.Generally prepared and used in the hydrochloride form as a white powder.Major active principle:lysozyme.Typical application:used as an antimicrobial in food processing. Pancreatin Obtained from porcine or bovine(ox)pancreatic tissue.Produced as a white to tan,water-soluble powder. Major active principles:(1)␣-amylase;(2)protease;and(3) lipase.Typical applications:used in the preparation of pre-cooked cereals,infant foods,and protein hydrolysates. Pepsin Obtained from the glandular layer of hog stomach. Produced as a white to light tan,water-soluble powder;amber paste;or clear,amber to brown,aqueous liquids.Major active principle:pepsin.Typical applications:used in the preparation of fishmeal and other protein hydrolysates and in the clotting of milk in manufacture of cheese(in combination with rennet). Phospholipase A2Obtained from porcine pancreatic tissue. Produced as a white to tan powder or pale to dark yellow liquid.Major active principle:phospholipase A2.Typical ap-plication:used in the hydrolysis of lecithins.Rennet,Bovine Aqueous extracts made from the fourth stomach of bovines.Produced as a clear,amber to dark brown liquid or a white to tan powder.Major active principle:prote-ase(pepsin).Typical application:used in the manufacture of cheese.Similar preparations may be made from the fourth stomach of sheep or goats.Rennet,Calf Aqueous extracts made from the fourth stom-ach of calves.Produced as a clear,amber to dark brown liquid or a white to tan powder.Major active principle:protease (chymosin).Typical application:used in the manufacture of cheese.Similar preparations may be made from the fourth stomach of lambs or kids.Trypsin Obtained from purified extracts of porcine or bo-vine pancreas.Produced as white to tan,amorphous powders soluble in water,but practically insoluble in alcohol,in chloro-form,and in ether.Major active principle:trypsin.Typical applications:used in baking,in the tenderizing of meat,and in the production of protein hydrolysates.Plant-Derived PreparationsAmylase Obtained from extraction of ungerminated barley. Produced as a clear,amber to dark brown liquid or a white to tan powder.Major active principle:-amylase.Typical applications:used in the production of alcoholic beverages and sugar syrups.Bromelain The purified proteolytic substance derived from the pineapples Ananas comosus and Ananas bracteatus L. (Fam.Bromeliaceae).Produced as a white to light tan,amor-phous powder soluble in water(the solution is usually color-less to light yellow and somewhat opalescent),but practically insoluble in alcohol,in chloroform,and in ether.Major active principle:bromelain.Typical applications:used in the chill-proofing of beer,in the tenderizing of meat,in the preparation of precooked cereals,in the production of protein hydroly-sates,and in baking.Ficin The purified proteolytic substance derived from the latex of Ficus sp.(Fam.Moraceae),which include a variety of tropical fig trees.Produced as a white to off white powder completely soluble in water.(Liquid fig latex concentrates are light to dark brown.)Major active principle:ficin.Typical applications:used in the chillproofing of beer,in the tenderiz-ing of meat,and in the conditioning of dough in baking. Malt The product of the controlled germination of barley. Produced as a clear amber to dark brown liquid preparations or as a white to tan powder.Major active principles:(1)␣-amylase and(2)-amylase.Typical applications:used in baking;used in the manufacture of alcoholic beverages and of syrups.Papain The purified proteolytic substance derived from the fruit of the papaya Carica papaya L.(Fam.Caricaceae).Pro-duced as a white to light tan,amorphous powder or a liquid soluble in water(the solution is usually colorless or light yellow and somewhat opalescent),but practically insoluble in alcohol,in chloroform,and in ether.Major active principles: (1)papain and(2)chymopapain.Typical applications:used in the chillproofing of beer,in the tenderizing of meat,in the148/Enzyme Preparations/Monographs FCC Vpreparation of precooked cereals,and in the production of protein hydrolysates.Microbially Derived Preparations␣-Acetolactatedecarboxylase(Bacillus subtilis containing a Bacillus brevis gene)Produced as a brown liquid by con-trolled fermentation using the modified Bacillus subtilis.Solu-ble in water(the solution is usually a light yellow to brown). Major active principle:decarboxylase.Typical application: used in the preparation of beer.Aminopeptidase,Leucine(Aspergillus niger var.,Aspergil-lus oryzae var.,and other microbial species)Produced as a light tan to brown powder or as a brown liquid by controlled fermentation using Aspergillus niger var.,Aspergillus oryzae var.,or other microbial species.The powder is soluble in water(the solution is usually light yellow to brown).Major active principles:(1)aminopeptidase,(2)protease,and(3) carboxypeptidase activities in varying amounts.Typical appli-cations:used in the preparation of protein hydrolysates and in the development of flavors in processed foods. Carbohydrase(Aspergillus niger var.,including Aspergillus aculeatus)Produced as an off white to tan powder or a tan to dark brown liquid by controlled fermentation using Aspergillus niger var.(including Aspergillus aculeatus).Solu-ble in water(the solution is usually light yellow to dark brown),but practically insoluble in alcohol,in chloroform, and in ether.Major active principles:(1)␣-amylase,(2)pec-tinase(a mixture of enzymes,including pectin depolymerase, pectin methyl esterase,pectin lyase,and pectate lyase),(3) cellulase,(4)glucoamylase(amyloglucosidase),(5)amylo-1,6-glucosidase,(6)hemicellulase(a mixture of enzymes, including poly(galacturonate)hydrolase,arabinosidase, mannosidase,mannanase,and xylanase),(7)lactase,(8)-glucanase,(9)-D-glucosidase,(10)pentosanase,and(11)␣-galactosidase.Typical applications:used in the preparation of starch syrups and dextrose,alcohol,beer,ale,fruit juices, chocolate syrups,bakery products,liquid coffee,wine,dairy products,cereals,and spice and flavor extracts. Carbohydrase(Aspergillus oryzae var.)Produced as an off white to tan,amorphous powder or a liquid by controlled fermentation using Aspergillus oryzae var.Soluble in water (the solution is usually light yellow to dark brown),but practi-cally insoluble in alcohol,in chloroform,and in ether.Major active principles:(1)␣-amylase,(2)glucoamylase(amyloglu-cosidase),and(3)lactase.Typical applications:used in the preparation of starch syrups,alcohol,beer,ale,bakery prod-ucts,and dairy products.Carbohydrase(Bacillus acidopullulyticus)Produced as an off white to brown,amorphous powder or a liquid by con-trolled fermentation using Bacillus acidopullulyticus.Soluble in water(the solution is usually light yellow to dark brown), but practically insoluble in alcohol,in chloroform,and in ether.Major active principle:pullulanase.Typical applica-tions:used in the hydrolysis of amylopectins and other branched polysaccharides.Carbohydrase(Bacillus stearothermophilus)Produced as an off white to tan powder or a light yellow to dark brown liquid by controlled fermentation using Bacillus stearother-mophilus.Soluble in water,but practically insoluble in alco-hol,in ether,and in chloroform.Major active principle:␣-amylase.Typical applications:used in the preparation of starch syrups,alcohol,beer,dextrose,and bakery products.Carbohydrase(Candida pseudotropicalis)Produced as an off white to tan,amorphous powder or a liquid by controlled fermentation using Candida pseudotropicalis.Soluble in water(the solution is usually light yellow to dark brown)but insoluble in alcohol,in chloroform,and in ether.Major active principle:lactase.Typical applications:used in the manufac-ture of candy and ice cream and in the modification of dairy products.Carbohydrase(Kluyveromyces marxianus ctis)Pro-duced as an off white to tan,amorphous powder or a liquid by controlled fermentation using Kluyveromyces marxianus ctis.Soluble in water(the solution is usually light yellow to dark brown),but insoluble in alcohol,in chloroform, and in ether.Major active principle:lactase.Typical applica-tions:used in the manufacture of candy and ice cream and in the modification of dairy products.Carbohydrase(Mortierella vinaceae var.raffinoseuti-lizer)Produced as an off white to tan powder or as pellets by controlled fermentation using Mortierella vinaceae var. raffinoseutilizer.Soluble in water(pellets may be insoluble in water),but practically insoluble in alcohol,in chloroform, and in ether.Major active principle:␣-galactosidase.Typical application:used in the production of sugar from sugar beets. Carbohydrase(Rhizopus niveus)Produced as an off white to brown,amorphous powder or a liquid by controlled fermen-tation using Rhizopus niveus.Soluble in water(the solution is usually light yellow to dark brown),but practically insoluble in alcohol,in chloroform,and in ether.Major active principles: (1)␣-amylase and(2)glucoamylase.Typical application:used in the hydrolysis of starch.Carbohydrase(Rhizopus oryzae var.)Produced as a pow-der or a liquid by controlled fermentation using Rhizopus oryzae var.Soluble in water,but practically insoluble in alco-hol,in chloroform,and in ether.Major active principles:(1)␣-amylase,(2)pectinase,and(3)glucoamylase(amylogluco-sidase).Typical applications:used in the preparation of starch syrups and fruit juices,vegetable purees,and juices and in the manufacture of cheese.Carbohydrase(Saccharomyces species)Produced as a white to tan,amorphous powder by controlled fermentation using a number of species of Saccharomyces traditionally used in the manufacture of food.Soluble in water(the solution is usually light yellow),but practically insoluble in alcohol, in chloroform,and in ether.Major active principles:(1)in-vertase and(2)lactase.Typical applications:used in the man-ufacture of candy and ice cream and in the modification of dairy products.FCC V Monographs/Enzyme Preparations/149Carbohydrase[(Trichoderma longibrachiatum var.)(for-merly reesei)]Produced as an off white to tan,amorphous powder or as a liquid by controlled fermentation using Tri-choderma longibrachiatum var.Soluble in water(the solution is usually tan to brown),but practically insoluble in alcohol, in chloroform,and in ether.Major active principles:(1)cellu-lase,(2)-glucanase,(3)-D-glucosidase,(4)hemicellulase, and(5)pentosanase.Typical applications:used in the prepara-tion of fruit juices,wine,vegetable oils,beer,and baked goods.Carbohydrase(Bacillus subtilis containing a Bacillus mega-terium␣-amylase gene)Produced as an off white to brown, amorphous powder or liquid by controlled fermentation using the modified Bacillus subtilis.Soluble in water(the solution is usually light yellow to dark brown),but practically insoluble in alcohol,in chloroform,and in ether.Major active principle:␣-amylase.Typical applications:used in the preparation of starch syrups,alcohol,beer,and dextrose.Carbohydrase(Bacillus subtilis containing a Bacillus stearo-thermophilus␣-amylase gene)Produced as an off white to brown,amorphous powder or a liquid by controlled fermenta-tion using the modified Bacillus subtilis.Soluble in water(the solution is usually light yellow to dark brown),but practically insoluble in alcohol,in chloroform,and in ether.Major active principle:maltogenic amylase.Typical applications:used in the preparation of starch syrups,dextrose,alcohol,beer,and baked goods.Carbohydrase and Protease,Mixed(Bacillus licheniformis var.)Produced as an off white to brown,amorphous powder or as a liquid by controlled fermentation using Bacillus licheni-formis var.Soluble in water(the solution is usually light yellow to dark brown),but practically insoluble in alcohol, in chloroform,and in ether.Major active principles:(1)␣-amylase and(2)protease.Typical applications:used in the preparation of starch syrups,alcohol,beer,dextrose,fishmeal, and protein hydrolysates.Carbohydrase and Protease,Mixed(Bacillus subtilis var. including Bacillus amyloliquefaciens)Produced as an off white to tan,amorphous powder or as a liquid by controlled fermentation using Bacillus subtilis var.Soluble in water(the solution is usually light yellow to dark brown),but practically insoluble in alcohol,in chloroform,and in ether.Major active principles:(1)␣-amylase,(2)-glucanase,(3)protease,and (4)pentosanase.Typical applications:used in the preparation of starch syrups,alcohol,beer,dextrose,bakery products,and fishmeal;in the tenderizing of meat;and in the preparation of protein hydrolysates.Catalase(Aspergillus niger var.)Produced as an off white to tan,amorphous powder or as a liquid by controlled fermen-tation using Aspergillus niger var.Soluble in water(the solu-tion is usually tan to brown),but practically insoluble in alcohol,in chloroform,and in ether.Major active principle: catalase.Typical applications:used in the manufacture of cheese,egg products,and soft drinks.Catalase(Micrococcus lysodeikticus)Produced by con-trolled fermentation using Micrococcus lysodeikticus.Soluble in water(the solution is usually light yellow to dark brown), but practically insoluble in alcohol,in chloroform,and in ether.Major active principle:catalase.Typical application: used in the manufacture of cheese,egg products,and soft drinks.Chymosin(Aspergillus niger var.awamori,Escherichia coli K-12,and Kluyveromyces marxianus,each microorganism containing a calf prochymosin gene)Produced as a white to tan,amorphous powder or as a light yellow to brown liquid by controlled fermentation using the above-named genetically modified microorganisms.The powder is soluble in water, but practically insoluble in alcohol,in chloroform,and in ether.Major active principle:chymosin.Typical application: used in the manufacture of cheese and in the preparation of milk-based desserts.Glucose Isomerase(Actinoplanes missouriensis,Bacillus co-agulans,Streptomyces olivaceus,Streptomyces olivochromo-genes,Microbacterium arborescens,Streptomyces rubigino-sus var.,or Streptomyces murinus)Produced as an off white to tan,brown,or pink,amorphous powder,granules,or liquid by controlled fermentation using any of the above-named organisms.The products may be soluble in water,but practi-cally insoluble in alcohol,in chloroform,and in ether;or if immobilized,may be insoluble in water and partially soluble in alcohol,in chloroform,and in ether.Major active principle: glucose(or xylose)isomerase.Typical applications:used in the manufacture of high-fructose corn syrup and other fructose starch syrups.Glucose Oxidase(Aspergillus niger var.)Produced as a yellow to brown solution or as a yellow to tan or off white powder by controlled fermentation using Aspergillus niger var.Soluble in water(the solution is usually light yellow to brown),but practically insoluble in alcohol,in chloroform, and in ether.Major active principles:(1)glucose oxidase and (2)catalase.Typical applications:used in the removal of sugar from liquid eggs and in the deoxygenation of citrus beverages.Lipase(Aspergillus niger var.)Produced as an off white to tan,amorphous powder by controlled fermentation using Aspergillus niger var.Soluble in water(the solution is usually light yellow),but practically insoluble in alcohol,in chloro-form,and in ether.Major active principle:lipase.Typical application:used in the hydrolysis of lipids(e.g.,fish oil concentrates and cereal-derived lipids).Lipase(Aspergillus oryzae var.)Produced as an off white to tan,amorphous powder or a liquid by controlled fermentation using Aspergillus oryzae var.Soluble in water(the solution is usually light yellow),but practically insoluble in alcohol, in chloroform,and in ether.Major active principle:lipase. Typical applications:used in the hydrolysis of lipids(e.g., fish oil concentrates)and in the manufacture of cheese and cheese flavors.150/Enzyme Preparations/Monographs FCC VLipase(Candida rugosa;formerly Candida cylindra-cea)Produced as an off white to tan powder by controlled fermentation using Candida rugosa.Soluble in water,but practically insoluble in alcohol,in chloroform,and in ether. Major active principle:lipase.Typical applications:used in the hydrolysis of lipids,in the manufacture of dairy products and confectionery goods,and in the development of flavor in processed foods.Lipase[Rhizomucor(Mucor)miehei]Produced as an off white to tan powder or as a liquid by controlled fermentation using Rhizomucor miehei.Soluble in water(the solution is usually light yellow to dark brown),but practically insoluble in alcohol,in chloroform,and in ether.Major active principle: lipase.Typical applications:used in the hydrolysis of lipids, in the manufacture of cheese,and in the removal of haze in fruit juices.Phytase(Aspergillus niger var.)Produced as an off white to brown powder or as a tan to dark brown liquid by controlled fermentation using Aspergillus niger var.Soluble in water, but practically insoluble in alcohol,in chloroform,and in ether.Major active principles:(1)3-phytase and(2)acid phosphatase.Typical applications:used in the production of soy protein isolate and in the removal of phytic acid from plant materials.Protease(Aspergillus niger var.)Produced by controlled fermentation using Aspergillus niger var.The purified enzyme occurs as an off white to tan,amorphous powder.Soluble in water(the solution is usually light yellow),but practically insoluble in alcohol,in chloroform,and in ether.Major active principle:protease.Typical application:used in the produc-tion of protein hydrolysates.Protease(Aspergillus oryzae var.)Produced by controlled fermentation using Aspergillus oryzae var.The purified en-zyme occurs as an off white to tan,amorphous powder.Soluble in water(the solution is usually light yellow),but practically insoluble in alcohol,in chloroform,and in ether.Major active principle:protease.Typical applications:used in the chill-proofing of beer,in the production of bakery products,in the tenderizing of meat,in the production of protein hydrolysates, and in the development of flavor in processed foods. Rennet,Microbial(nonpathogenic strain of Bacillus ce-reus)Produced as a white to tan,amorphous powder or a light yellow to dark brown liquid by controlled fermentation using Bacillus cereus.Soluble in water,but practically insolu-ble in alcohol,in chloroform,and in ether.Major active princi-ple:protease.Typical application:used in the manufacture of cheese.Rennet,Microbial(Endothia parasitica)Produced as an off white to tan,amorphous powder or as a liquid by controlled fermentation using nonpathogenic strains of Endothia parasit-ica.The powder is soluble in water(the solution is usually tan to dark brown),but practically insoluble in alcohol,in chloroform,and in ether.Major active principle:protease. Typical application:used in the manufacture of cheese.Rennet,Microbial[Rhizomucor(Mucor)sp.]Produced as a white to tan,amorphous powder by controlled fermentation using Rhizomucor miehei,or pusillus var.Lindt.The powder is soluble in water(the solution is usually light yellow),but practically insoluble in alcohol,in chloroform,and in ether. Major active principle:protease.Typical application:used in the manufacture of cheese.Transglutaminase(Streptoverticillium mobaraense var.) Produced as an off white to weak yellow-brown,amorphous powder by controlled fermentation using Streptoverticillium mobaraense var.Soluble in water but practically insoluble in alcohol,in chloroform,and in ether.Major active principle: transglutaminase.Typical applications:used in the processing of meat,poultry,and seafood;production of yogurt,certain cheeses,and frozen desserts;and manufacture of pasta prod-ucts and noodles,baked goods,meat analogs,ready-to-eat cereals,and other grain-based foods.REACTIONS CATALYZEDNote:The reactions catalyzed by any given active com-ponent are essentially the same,regardless of the sourcefrom which that component is derived.␣-Acetolactatedecarboxylase Decarboxylation of␣-aceto-lactate to acetoin.Aminopeptidase,Leucine Hydrolysis of N-terminal amino acid,which is preferably leucine,but may be other amino acids,from proteins and oligopeptides,yielding free amino acids and oligopeptides of lower molecular weight.␣-Amylase Endohydrolysis of␣-1,4-glucan bonds in poly-saccharides(starch,glycogen,etc.),yielding dextrins and ol-igo-and monosaccharides.-Amylase Hydrolysis of␣-1,4-glucan bonds in polysac-charides(starch,glycogen,etc.),yielding maltose and beta-limit dextrins.Bromelain Hydrolysis of polypeptides,amides,and esters (especially at bonds involving basic amino acids,leucine,or glycine),yielding peptides of lower molecular weight. Catalase2H2O2→O2+2H2O.Cellulase Hydrolysis of-1,4-glucan bonds in such poly-saccharides as cellulose,yielding-dextrins.Chymosin(calf and fermentation derived)Cleaves a single bond in kappa casein.Ficin Hydrolysis of polypeptides,amides,and esters(espe-cially at bonds involving basic amino acids,leucine,or gly-cine),yielding peptides of lower molecular weight.␣-Galactosidase Hydrolysis of terminal nonreducing␣-D-galactose residues in␣-D-galactosides.-Glucanase Hydrolysis of-1,3-and-1,4-linkages in-D-glucans,yielding oligosaccharides and glucose.FCC V Monographs/Enzyme Preparations/151Glucoamylase(amyloglucosidase)Hydrolysis of terminal ␣-1,4-and␣-1,6-glucan bonds in polysaccharides(starch, glycogen,etc.),yielding glucose(dextrose).Glucose Isomerase(xylose isomerase)Isomerization of glucose to fructose,and xylose to xylulose.Glucose Oxidase-D-glucose+O2→D-glucono-␦-lactone +H2O2.-D-Glucosidase Hydrolysis of terminal,nonreducing-D-glucose residues with the release of-D-glucose. Hemicellulase Hydrolysis of-1,4-glucans,␣-L-arabino-sides,-D-mannosides,1,3--D-xylans,and other polysaccha-rides,yielding polysaccharides of lower molecular weight. Invertase(-fructofuranosidase)Hydrolysis of sucrose to a mixture of glucose and fructose(invert sugar).Lactase(-galactosidase)Hydrolysis of lactose to a mixture of glucose and galactose.Lysozyme Hydrolysis of cell-wall polysaccharides of vari-ous bacterial species leading to the breakdown of the cell wall most often in Gram-positive bacteria.Maltogenic Amylase Hydrolysis of␣-1,4-glucan bonds. Lipase Hydrolysis of triglycerides of simple fatty acids, yielding mono-and diglycerides,glycerol,and free fatty acids. Pancreatin␣-Amylase Hydrolysis of␣-1,4-glucan bonds. Protease Hydrolysis of proteins and polypepticles. Lipase Hydrolysis of triglycerides of simple fatty acids. PectinasePectate lyase Hydrolysis of pectate to oligosaccharides. Pectin depolymerase Hydrolysis of1,4-galacturonide bonds.Pectin lyase Hydrolysis of oligosaccharides formed by pectate lyase.Pectinesterase Demethylation of pectin.Pepsin Hydrolysis of polypeptides,including those with bonds adjacent to aromatic or dicarboxylic L-amino acid resi-dues,yielding peptides of lower molecular weight. Phospholipase A2Hydrolysis of lecithins and phosphatidyl-choline,producing fatty acid anions.Phytase3-Phytase myo-Inositol hexakisphosphate+H2O→1,2,4, 5,6-pentakisphosphate+orthophosphate.Acid Phosphatase Orthophosphate monoester+H2O→an alcohol+orthophosphate.Protease(generic)Hydrolysis of polypeptides,yielding peptides of lower molecular weight.Pullulanase Hydrolysis of1,6-␣-D-glycosidic bonds on amylopectin and glycogen and in␣-and-limit dextrins, yielding linear polysaccharides.Rennet(bovine and calf)Hydrolysis of polypeptides;speci-ficity may be similar to pepsin.Transglutaminase Binding of proteins.Trypsin Hydrolysis of polypeptides,amides,and esters at bonds involving the carboxyl groups of L-arginine and L-lysine,yielding peptides of lower molecular weight. GENERAL REQUIREMENTSEnzyme preparations are produced in accordance with good manufacturing practices.Regardless of the source of deriva-tion,they should cause no increase in the total microbial count in the treated food over the level accepted for the respective food.Animal tissues used to produce enzymes must comply with the applicable U.S.meat inspection requirements and must be handled in accordance with good hygienic practices. Plant material used to produce enzymes or culture media used to grow microorganisms consist of components that leave no residues harmful to health in the finished food under normal conditions of use.Preparations derived from microbial sources are produced by methods and under culture conditions that ensure a con-trolled fermentation,thus preventing the introduction of mi-croorganisms that could be the source of toxic materials and other undesirable substances.The carriers,diluents,and processing aids used to produce the enzyme preparations shall be substances that are accept-able for general use in foods,including water and substances that are insoluble in foods but removed from the foods after processing.Although limits have not been established for mycotoxins, appropriate measures should be taken to ensure that the prod-ucts do not contain such contaminants.ADDITIONAL REQUIREMENTSAssay Not less than85.0%and not more than115.0%of the declared units of enzyme activity.Lead Not more than5mg/kg.Microbial Limits:Coliforms Not more than30CFU per gram. Salmonella Negative in25g.TESTSAssay The following procedures,which are included under Enzyme Assays,Appendix V,are provided for application as necessary in determining compliance with the declared。
美国药典在线查询美国药典USP
美国药典在线查询美国药典USP导读：就爱阅读网友为您分享以下“美国药典USP”资讯，希望对您有所帮助，感谢您对的支持!美国药典USP浓度重量克分子浓度、容量克分子浓度和当量浓度用于本药典内大部分化学含量测定和检测方法中（亦见容量溶液于试剂、指示剂和溶液篇章中）重量克分子浓度用m表示，前面有一个数目字即为该溶质的克分子数（1公斤的所标明的溶液中）容量克分子浓度用M表示，前面的数目字表示在制备1立升溶液中所含的该溶质的克分子数当量浓度用N表示，前面的数目字表示制备1立升溶液中该溶质的克当量数。
百分比计量—百分比浓度如下表示：重量于重量百分比—（w/w）表示一个组分在100克溶液或混合物中的克数重量于容量百分比—（w/v）表示一个组分在100毫升溶液中的毫升数（不管溶剂是水还是其他液体）容量于容量百分比—（v/v）表示一个组分在100毫升溶液中的毫升数用百分比这个名词没有限定意义，对固体和半固体用w/w；对溶液或固体在溶液中的悬浮液用w/v；对液体在液体溶液用v/v；气体在液体内用w/v，例：一个1%的溶液是由溶解1克固体或半固体或1毫升溶液于足够的溶剂使成100毫升溶液。
由于室温的差异，微小的容量计量差异可忽略。
有效数据和允许偏差此处表示的数限是上限和下限并包括此二值以及其间的所有数字，但在限度以外的数值不在内。
在供试品的专篇内，检测中不管数字是以百分比还是绝对数字来表示都是表示最末的数字。
在容量滴定法中相当的叙述——容量滴定法故采用包括相当于标化滴定液的每毫升相当于供试品的重量，在这样的相当陈述，滴定液的浓度中的有效数字被认为相当于供试品的重量有效数字，所有的容量滴定应做空白校正。
允许偏差—药典所述的供试品的专篇内所规定的那些限度的建立是把供试品作为药物来使用或作为营养剂、饮食补充剂使用，除非另有其他指定。
药物的活性成分用分子式来计其强度标明了化学本质，如同已给的供试品的化学全名其绝对纯度为100%。
(完整版)美国药典USP31(921)翻译版(上)
(921 ) WATER DETERMINATION 水分测定Many Pharmacopeial articles either are hydrates or contain water in adsorbed form. As a result, the determination of the water content is important in demonstrating compliance with thePharmacopeial standards. Generally one of the methods given below is called for in the individual monograph, depending upon the nature of the article. In rare cases, a choice is allowed between two methods. When the article contains water of hydration, the Method I (Titrimetric), the Method II (Azeotropic), or the Method III (Gravimetric) is employed, as directed in the individual monograph, and the requirement is given under the heading Water.很多药典物品要么是水合物,要么含有处丁吸附状态的水.因此,测定水分含量对丁证实与药典标准的符合性是很重要的.通常,在具体的各论中会根据该物品的性质,要求使用下面假设干方法中的一个. 偶尔,会允许在2个方法中任选一个.当该物品含有水合状态的水,根据具体各论中的规定,使用方法I (滴定测量法)、方法II (包沸测量法)、或方法III (重量分析法),这个要求在标题水分项下给出.The heading Loss on drying (see Loss on Drying 731 ) is used in those cases where the loss sustained on heating may be not entirely water.在加热时的持续失重可能不全是水分的情况下,使用标题枯燥失重(见十燥失重<731>).METHOD I (TITRIMETRIC) 方法I (滴定测量法)Determine the water by Method Ia, unless otherwise specified in the individual monograph. 除非具体各论中另有规定,使用方法Ia来测定水分.Method Ia (Direct Titration) 方法Ia (直接滴定)Principle — The titrimetric determination of water is based upon the quantitative reaction of water with an anhydrous solution of sulfur dioxide and iodine in the presence of a buffer that reacts with hydrogen ions.原理：水分的滴定法检测是基丁水与二氧化硫的无水溶液以及存在丁缓冲液中与氢离子反响的碘之间的定量反响.In the original titrimetric solution, known as Karl Fischer Reagent, the sulfur dioxide and iodine are dissolved in pyridine and methanol. The test specimen may be titrated with the Reagent directly, or the analysis may be carried out by a residual titration procedure. The stoichiometry of the reactionis not exact, and the reproducibility of a determination depends upon such factors as the relativeconcentrations of the Reagent ingredients, the nature of the inert solvent used to dissolve the test specimen, and the technique used in the particular determination. Therefore, an empirically standardized technique is used in order to achieve the desired accuracy. Precision in the method is governed largely by the extent to which atmospheric moisture is excluded from the system. The titration of water is usually carried out with the use of anhydrous methanol as the solvent for the test specimen; however, other suitable solvents may be used for special or unusual test specimens. 在最初的滴定测量溶液〔即卡尔•费休试剂〕中,二氧化硫和碘溶解于嚅噬和甲醇中.该供试样品可以用该试剂直接滴定,或者可以使用残留滴定程序来进行该分析. 此反响的化学计算法不够准确,并且检测的重现性取决于某些因素,例如该试剂成分的相对浓度、用于溶解供试样品的惰性溶剂的性质、用于具体测定的方法等.因此,需要应用根据经验得到的标准化方法,以便实现预期的准确性.该方法中的精密度很大程度上取决于将大气湿度从该系统中排除的程度. 进行水分滴定通常使用无水甲醇作为供试样品的溶剂；但是,可以将其他适当的溶剂用于特殊或不常见的供试样品.Apparatus — Any apparatus may be used that provides for adequate exclusion of atmospheric moisture and determination of the endpoint. In the case of a colorless solution that is titrated directly, the endpoint may be observed visually as a change in color from canary yellow to amber. The reverse is observed in the case of a test specimen that is titrated residually. More commonly, however, the endpoint is determined electrometrically with an apparatus employing a simple electrical circuit that serves to impress about 200 mV of applied potential between a pair of platinum electrodes immersed in the solution to be titrated. At the endpoint of the titration a slight excess of the reagent increases the flow of current to between 50 and 150 microamperes for 30 seconds to 30 minutes, depending upon the solution being titrated. The time is shortest for substances that dissolve in the reagent. With some automatic titrators, the abrupt change in current or potential at the endpoint serves to close a solenoid-operated valve that controls the buret delivering the titrant. Commercially available apparatus generally comprises a closed system consisting of one or two automatic burets and a tightly covered titration vessel fitted with the necessary electrodes and a magnetic stirrer. The air in the system is kept dry with a suitable desiccant, and the titration vessel may be purged by means of a stream of dry nitrogen or current of dry air.仪器：任何能够充分排除大气湿度,并能测定终点的仪器.在直接向无色溶液滴定的情况下,可以通过从淡黄色到琥珀色的颜色改变来观察此终点. 在向供试样品作残留滴定的情况下, 会观察到与此相反的情况.但是,更常见的情况是,使用仪器,利用其中的简单电路在浸没在待滴定溶液中的一对白金电极上加上200mV的应用电压,从而以电势滴定来测定终点.在滴定终点,稍微过量的该试剂会使电流提升到50和150微安培,并维持30秒到30分钟,具体时间取决于被滴定的溶液. 溶解于该试剂中的物质所用时间是最短的. 在一些自动滴定仪上,在该终点出现的电流或电压的忽然变化会使由螺线管操纵的阀门关闭,该阀门限制者输送滴定剂的滴定管. 市场上销售的仪器通常包含一个封闭系统,其中由一个或两个自动滴定管、一个配备了必须的电极和磁力搅拌器的严密覆盖的滴定容器组成.通过适当的十燥器使系统内空气保持十燥, 并且该滴定容器可以通过十燥氮气流或十燥空气流来进行净化.Reagent — Prepare the Karl Fischer Reagent as follows. Add 125 g of iodine to a solution containing 670 mL of methanol and 170 mL of pyridine, and cool. Place 100 mL of pyridine in a 250-mL graduated cylinder, and, keeping the pyridine cold in an ice bath, pass in dry sulfur dioxide until the volume reaches 200 mL. Slowly add this solution, with shaking, to the cooled iodine mixture. Shake to dissolve the iodine, transfer the solution to the apparatus, and allow the solution to stand overnight before standardizing. One mL of this solution when freshly prepared is equivalent to approximately 5 mg of water, but it deteriorates gradually; therefore, standardize it within 1 hour before use, or daily if in continuous use. Protect from light while in use. Store any bulk stock of the reagent in a suitably sealed, glass-stoppered container, fully protected from light, and under refrigeration.试剂：按下面方法配制卡尔•费休试剂.参加125克碘至含有670mL甲醇和170mL嚅噬的溶液中, 放凉.将100mL嚅噬置于一个250mL量筒中,将该嚅噬置于冰浴中以保持冰冷,送入十燥二氧化硫直到体积到达200mL.伴随摇动,缓慢将此溶液参加到放凉后的碘混合物中.摇动以使碘溶解, 转移此溶液至该仪器,并在标准化之前将该溶液静置过夜.在刚刚配制之后, 1mL此溶液相当于约5mg水,但是会逐渐变差；因此,在使用前1个小时,或在连续使用时每日,对其进行标准化.使用中需避光.将该试剂的散装存货保存于适当密闭的玻璃塞容器中,完全避光,并冷藏.A commercially available, stabilized solution of Karl Fischer type reagent may be used. Commercially available reagents containing solvents or bases other than pyridine or alcohols other than methanol may be used also. These may be single solutions or reagents formed in situ by combining the components of the reagents present in two discrete solutions. The diluted Reagent called for in some monographs should be diluted as directed by the manufacturer. Either methanol or other suitable solvent, such as ethylene glycol monomethyl ether, may be used as the diluent.可以使用市场上销售的卡尔•费休类型试剂的稳定溶液.也可以使用市场上销售的试剂,其中含有除了嚅噬之外的溶剂或盐基,或除了甲醇之外的醇类.这些可以是通过合并存在于两个独立溶液中的试剂组成局部,在现场形成的单一的溶液或试剂.如果某些各论中要求使用稀释后的试剂,那么应当根据生产商的规定稀释.可以使用甲醇或其他适当溶剂,例如乙二醇一甲酰,作为稀释剂.Test Preparation — Unless otherwise specified in the individual monograph, use an accurately weighed ormeasured amount of the specimen under test estimated to contain 2 to 250 mg of water. The amount of water depends on the water equivalency factor of the Reagent and on the method of endpoint determination. In most cases, the minimum amount of specimen, in mg, can be estimated using the formula:供试配制品：除非在具体各论中另有规定,使用数量经过精确称定或称量的供试样品,其中应含水2至250mg.水的数量取决丁试剂的水当量因子和终点测定的方法.在大多数情况下,可以使用此公式估计以毫克计的供试样品的最小量：FCV/KFin which F is the water equivalency factor of the Reagent, in mg per mL; C is the used volume, in percent, of the capacity of the buret; V is the buret volume, in mL; and KF is the limit or reasonable expected water content in the sample, in percent. C is between 30% and 100% for manual titration, and between 10% and 100% for the instrumental method endpoint determination. 其中,F是试剂的水当量因子,单位为毫克每毫升；C是滴定管容量中所使用的体积〔为白分比〕；V是滴定管体积,以毫升计；KF是样品中限度或合理预期的水含量,为白分比.对丁手动滴定, C 值在30%至100%之间,而对丁仪器方法终点测定,其在10%至100%之间.Where the specimen under test is an aerosol with propellant, store it in a freezer for not less than 2 hours, open the container, and test 10.0 mL of the well-mixed specimen. In titrating the specimen,□determine the endpoint at a temperature of 10 or higher.如果供试样品是带有推进剂的气雾剂〔烟雾剂、气溶胶〕,将其存放丁冷冻室中不少丁2小时,翻开容器,并检验10.0mL混合均匀的样品.在滴定该样品过程中,在10口或更高的温度下确定反响终点.Where the specimen under test is capsules, use a portion of the mixed contents of not fewer than 4 capsules. 如果该供试样品为胶囊,使用不少丁4个胶囊的混合内容物的一局部.Where the specimen under test is tablets, use powder from not fewer than 4 tablets ground to a fine powder in an atmosphere of temperature and relative humidity known not to influence the results.如果该供试品为片剂,在不会影响检验结果的温度和相对湿度环境中, 将不少丁4片磨碎至细粉末.Where the monograph specifies that the specimen under test is hygroscopic, use a dry syringe to inject an appropriate volume of methanol, or other suitable solvent, accurately measured, into a tared container, and shake to dissolve the specimen. Using the same syringe, remove the solution from the container and transferit to a titration vessel prepared as directed for Procedure. Repeat the procedure with a second portion of methanol, or other suitable solvent, accurately measured, add this washing to the titration vessel, and immediately titrate. Determine the water content, in mg, of a portion of solvent of the same total volume as that used to dissolve the specimen and to wash the container and syringe, as directed for Standardization of Water Solution for Residual Titrations, and subtract this value from the water content, in mg, obtained in the titration of the specimen underotest. Dry the container and its closure at 100 for 3 hours, allow to cool in a desiccator, and weigh. Determine the weight of specimen tested from the difference in weight from the initial weight of the container.如果该各论中显示此供试样品易吸湿, 使用一个枯燥注射器,注射经过精确称量的适当体积的甲醇或其他适当溶剂,至一个已称过皮重的容器,并摇动以使该样品溶解.使用同一个注射器,从该容器中吸出此溶液并转移至根据步骤项下规定准备的一个滴定容器.使用精确称量的第二局部甲醇或其他适当溶剂,重复该步骤,将此洗液参加至滴定容器,并马上滴定.取与用丁溶解样品以及洗涤容器和注射器的溶剂同样体积的一局部溶剂, 根据用丁残留滴定的水溶液的标准化项下的规定,测定溶剂中的水分含量〔以mg为单位〕,并从得自供试样品滴定的水分含量〔以mg为单位〕中减去此数值.在100“温度条件下将这些容器及其盖子枯燥3小时,在枯燥器中静置至凉,并称重.根据与该容器初始重量的差距,来确定试验所用的样品重量.Standardization of the Reagent ——Place enough methanol or other suitable solvent in the titration vessel to cover the electrodes, and add sufficient Reagent to give the characteristic endpoint color, or 100 50 microamperes of direct current at about 200 mV of applied potential.试剂的标准化：将足够的甲醇或其他适当溶剂置丁滴定容器,以覆盖电极,并参加充足的试剂,以产生典型终点颜色,或者在约200mV应用电压下产生100 土50微安培直流电.For determination of trace amounts of water 〔less than 1%〕, it is preferable to use waterReagent with a equivalency factor of not more than 2.0. Sodium tartrate may be used as a convenient waterreference substance. Quickly add 75 to 125 mg of sodium tartrate 〔C 4H4Na2Q e 2H2O〕, accurately weighed by difference, and titrate to the endpoint. The water equivalence factor F, in mg of water per mL of reagent, is given by the formula:为了检测痕量水份〔少丁1%〕最好使用水当量因子不超过 2.0的试剂.可以使用洒石酸钠作为便捷的水标准物质.快速参加精密称定的75至125mg洒石酸钠〔C4H4Na2Q e 2H2O〕,并滴定至终点. 在下面的公式中给出了水平■衡因子F的计算方法〔单位为以每毫升试剂中毫克水〕：2〔18.02/230.08〕〔 W/V〕,in which 18.02 and 230.08 are the molecular weights of water and sodium tartrate dihydrate, respectively; W is the weight, in mg, of sodium tartrate dihydrate; and V is the volume, in mL, of the Reagent consumed in the second titration.其中,18.02和230.08是水和洒石酸钠二水合物的分子量；W是洒石酸钠二水合物的重量〔单位mg〕; V是第二次滴定中消耗的试剂体积〔单位mL〕.For the precise determination of significant amounts of water 〔1% or more〕, use Purified Water as the reference substance. Quickly add between 25 and 250 mg of water, accurately weighed by difference, from a weighing pipet or from a precalibrated syringe or micropipet, the amount taken being governed by the reagent strength and the buret size, as referred to under VolumetricApparatus 31 . Titrate to the endpoint. Calculate the water equivalence factor, F, in mg of water per mL of reagent, by the formula:为了精确测定显著水分含量〔1%或更多〕,使用纯洁水作为标准物质.从称重移液器或者经过预校准的注射器或微量移液器中,快速参加经过精密称定的25至50mg水,参加数量需取决丁该试剂的水平和滴定管的大小,参见称量器具＜31＞.滴定至终点.使用下面公式,计算水分平衡因子 F 〔单位为每毫升试剂中毫克水〕.W/V,in which W is the weight, in mg, of the water; and V is the volume, in mL, of the reagent required. 其中W是水的重量〔单位mg〕 ; V是需要的试剂体积〔单位mL〕.Procedure — Unless otherwise specified, transfer 35 to 40 mL of methanol or other suitable solvent to the titration vessel, and titrate with the Reagent to the electrometric or visual endpoint to consume any moisture that may be present. 〔Disregard the volume consumed, since it does not enter into the calculations.〕Quickly add the Test Preparation, mix, and again titrate with theReagent to the electrometric or visual endpoint. Calculate the water content of the specimen, in mg, taken by the formula:步骤：除非另有规定,转移35至40mL甲醇或其他适当溶剂至滴定容器,并使用该试剂进行滴定至测电法或视觉观察的终点,以消耗掉可能存在的任何水分. 〔不要理会消耗的体积,由于其不会带入计算.〕快速参加供试配制液,混匀,并再次使用试剂滴定至测电法或视觉观察的终点.使用下面的公式,计算样品中的水分含量：SF,in which S is the volume, in mL, of the Reagent consumed in the second titration; and F is the water equivalence factor of the Reagent.其中,S是在第二次滴定中消耗掉的试剂体积〔单位mL〕 ; F是该试剂的水平衡因子.。
美国药典USP31无菌检查
美国药典USP31-NF26无菌检查法《71》.doc71 STERILITY TESTS 无菌检查法Portions of this general chapter have been harmonized with the corresponding texts of the European Pharmacopeia and/or the Japanese Pharmacopeia. Those portions that are not harmonized are marked with symbols () to specify this fact.此通则的各部分已经与欧洲药典和/或日本药典的对应部分做了协调。
不一致的部分用符号（）来标明。
The following procedures are applicable for determining whether a Pharmacopeial article purporting to be sterile complies with the requirements set forth in the individual monograph with respect to the test for sterility. Pharmacopeial articles are to be tested by the Membrane Filtration method under Test for Sterility of the Product to be Examined where the nature of the product permits. If the membrane filtration technique is unsuitable, use the Direct Inoculation of the Culture Medium method under Test for Sterility of the Product to be Examined. All devices, with the exception of Devices with Pathways Labeled Sterile, are tested using the Direct Inoculation of the Culture Medium method. Provisions for retesting are included under Observation and Interpretation of Results.下面这些步骤适用于测定是否某个用于无菌用途的药品是否符合其具体的各论中关于无菌检查的要求。
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921WATER DETERMINATION水分测定Many Pharmacopeial articles either are hydrates or contain water in adsorbed form. As a result, the determination of the water content is important in demonstrating compliance with the Pharmacopeial standards. Generally one of the methods given below is called for in the individual monograph, depending upon the nature of the article. In rare cases, a choice is allowed between two methods. When the article contains water of hydration, the Method I (Titrimetric), the Method II (Azeotropic), or the Method III (Gravimetric) is employed, as directed in the individual monograph, and the requirement is given under the heading Water.很多药典物品要么是水合物，要么含有处于吸附状态的水。
因此，测定水分含量对于证实与药典标准的符合性是很重要的。
通常，在具体的各论中会根据该物品的性质，要求使用下面若干方法中的一个。
偶尔，会允许在2个方法中任选一个。
当该物品含有水合状态的水，按照具体各论中的规定，使用方法I（滴定测量法）、方法II（恒沸测量法）、或方法III（重量分析法），这个要求在标题水分项下给出。
The heading Loss on drying (see Loss on Drying 731) is used in those cases where the loss sustained on heating may be not entirely water.在加热时的持续失重可能不全是水分的情况下，使用标题干燥失重（见干燥失重<731>）。
METHOD I (TITRIMETRIC) 方法I（滴定测量法）Determine the water by Method Ia, unless otherwise specified in the individual monograph.除非具体各论中另有规定，使用方法Ia来测定水分。
Method Ia (Direct Titration) 方法Ia（直接滴定）Principle— The titrimetric determination of water is based upon the quantitative reaction of water with an anhydrous solution of sulfur dioxide and iodine in the presence of a buffer that reacts with hydrogen ions.原理：水分的滴定法检测是基于水与二氧化硫的无水溶液以及存在于缓冲液中与氢离子反应的碘之间的定量反应。
In the original titrimetric solution, known as Karl Fischer Reagent, the sulfur dioxide and iodine are dissolved in pyridine and methanol. The test specimen may be titrated with the Reagent directly, or the analysis may be carried out by a residual titration procedure. The stoichiometry of the reactionis not exact, and the reproducibility of a determination depends upon such factors as the relative concentrations of the Reagent ingredients, the nature of the inert solvent used to dissolve the test specimen, and the technique used in the particular determination. Therefore, an empirically standardized technique is used in order to achieve the desired accuracy. Precision in the method is governed largely by the extent to which atmospheric moisture is excluded from the system. The titration of water is usually carried out with the use of anhydrous methanol as the solvent for the test specimen; however, other suitable solvents may be used for special or unusual test specimens.在最初的滴定测量溶液（即卡尔·费休试剂）中，二氧化硫和碘溶解于嘧啶和甲醇中。
该供试样品可以用该试剂直接滴定，或者可以使用残留滴定程序来进行该分析。
此反应的化学计算法不够准确，并且检测的重现性取决于某些因素，例如该试剂成分的相对浓度、用于溶解供试样品的惰性溶剂的性质、用于具体测定的方法等。
因此，需要应用根据经验得到的标准化方法，以便实现预期的准确性。
该方法中的精密度很大程度上取决于将大气湿度从该系统中排除的程度。
进行水分滴定通常使用无水甲醇作为供试样品的溶剂；但是，可以将其他适当的溶剂用于特殊或不常见的供试样品。
Apparatus— Any apparatus may be used that provides for adequate exclusion of atmospheric moisture and determination of the endpoint. In the case of a colorless solution that is titrated directly, the endpoint may be observed visually as a change in color from canary yellow to amber. The reverse is observed in the case of a test specimen that is titrated residually. More commonly, however, the endpoint is determined electrometrically with an apparatus employing a simple electrical circuit that serves to impress about 200 mV of applied potential between a pair of platinum electrodes immersed in the solution to be titrated. At the endpoint of the titration a slight excess of the reagent increases the flow of current to between 50 and 150 microamperes for 30 seconds to 30 minutes, depending upon the solution being titrated. The time is shortest for substances that dissolve in the reagent. With some automatic titrators, the abrupt change in current or potential at the endpoint serves to close a solenoid-operated valve that controls the buret delivering the titrant. Commercially available apparatus generally comprises a closed system consisting of one or two automatic burets and a tightly covered titration vessel fitted with the necessary electrodes and a magnetic stirrer. The air in the system is kept dry with a suitable desiccant, and the titration vessel may be purged by means of a stream of dry nitrogen or current of dry air.仪器：任何能够充分排除大气湿度，并能测定终点的仪器。
在直接向无色溶液滴定的情况下，可以通过从淡黄色到琥珀色的颜色改变来观察此终点。
在向供试样品作残留滴定的情况下，会观察到与此相反的情况。
但是，更常见的情况是，使用仪器，利用其中的简单电路在浸没在待滴定溶液中的一对白金电极上加上200mV的应用电压，从而以电势滴定来测定终点。
在滴定终点，轻微过量的该试剂会使电流提高到50和150微安培，并维持30秒到30分钟，具体时间取决于被滴定的溶液。
溶解于该试剂中的物质所用时间是最短的。