Lixivaptan_LCMS_25740_MedChemExpress
Gelucire-14-44-SDS-MedChemExpress
Inhibitors, Agonists, Screening LibrariesSafety Data Sheet Revision Date:Nov.-23-2018Print Date:Nov.-23-20181. PRODUCT AND COMPANY IDENTIFICATION1.1 Product identifierProduct name :Gelucire 14/44Catalog No. :HY-Y1892CAS No. :121548-04-71.2 Relevant identified uses of the substance or mixture and uses advised againstIdentified uses :Laboratory chemicals, manufacture of substances.1.3 Details of the supplier of the safety data sheetCompany:MedChemExpress USATel:609-228-6898Fax:609-228-5909E-mail:sales@1.4 Emergency telephone numberEmergency Phone #:609-228-68982. HAZARDS IDENTIFICATION2.1 Classification of the substance or mixtureNot a hazardous substance or mixture.2.2 GHS Label elements, including precautionary statementsNot a hazardous substance or mixture.2.3 Other hazardsNone.3. COMPOSITION/INFORMATION ON INGREDIENTS3.1 SubstancesSynonyms:NoneFormula:N/AMolecular Weight:N/ACAS No. :121548-04-74. 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PHYSICAL AND CHEMICAL PROPERTIES9.1 Information on basic physical and chemical propertiesAppearance White to off-white (Oil)Odor No data availableOdor threshold No data availablepH No data availableMelting/freezing point No data availableBoiling point/range No data availableFlash point No data availableEvaporation rate No data availableFlammability (solid, gas)No data availableUpper/lower flammability or explosive limits No data availableVapor pressure No data availableVapor density No data availableRelative density No data availableWater Solubility No data availablePartition coefficient No data availableAuto-ignition temperature No data availableDecomposition temperature No data availableViscosity No data availableExplosive properties No data availableOxidizing properties No data available9.2 Other safety informationNo data available.10. 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marked manuscript
Quality evaluation of Flos Lonicerae through a simultaneous determination of seven saponins by HPLC with ELSDXing-Yun Chai1, Song-Lin Li2, Ping Li1*1Key Laboratory of Modern Chinese Medicines and Department of Pharmacognosy, China Pharmaceutical University, Nanjing, 210009, People’s Republic of China2Institute of Nanjing Military Command for Drug Control, Nanjing, 210002, People’s Republic of China*Corresponding author: Ping LiKey Laboratory of Modern Chinese Medicines and Department of Pharmacognosy, China Pharmaceutical University, Nanjing 210009, People’s Republic of China.E-mail address: lipingli@Tel.: +86-25-8324-2299; 8539-1244; 135********Fax: +86-25-8532-2747AbstractA new HPLC coupled with evaporative light scattering detection (ELSD) method has been developed for the simultaneous quantitative determination of seven major saponins, namely macranthoidinB (1), macranthoidin A (2), dipsacoside B (3), hederagenin-28-O-β-D-glucopyranosyl(6→1)-O-β-D- glucopyranosyl ester (4), macranthoside B (5), macranthoside A (6), and hederagenin-3-O-α-L-arabinopyranosyl(2→1)-O-α-L-rhamnopyranoside (7)in Flos Lonicerae, a commonly used traditional Chinese medicine (TCM) herb.Simultaneous separation of these seven saponins was achieved on a C18 analytical column with a mixed mobile phase consisting of acetonitrile(A)-water(B)(29:71 v/v) acidified with 0.5% acetic acid. The elution was operated from keeping 29%A for 10min, then gradually to 54%B from 10 to 25 min on linear gradient, and then keep isocratic elution with 54%B from 25 to 30min.The drift tube temperature of ELSD was set at 106℃, and with the nitrogen flow-rate of 2.6 l/min. All calibration curves showed good linear regression (r2 0.9922) within test ranges. This method showed good reproducibility for the quantification of these seven saponins in Flos Lonicerae with intra- and inter-day variations of less than 3.0% and 6.0% respectively. The validated method was successfully applied to quantify seven saponins in five sources of Flos Lonicerae, which provides a new basis of overall assessment on quality of Flos Lonicerae.Keywords: HPLC-ELSD; Flos Lonicerae; Saponins; Quantification1. IntroductionFlos Lonicerae (Jinyinhua in Chinese), the dried buds of several species of the genus Lonicera (Caprifoliaceae), is a commonly used traditional Chinese medicine (TCM) herb. It has been used for centuries in TCM practice for the treatment of sores, carbuncles, furuncles, swelling and affections caused by exopathogenic wind-heat or epidemic febrile diseases at the early stage [1]. Though four species of Lonicera are documented as the sources of Flos Lonicerae in China Pharmacopeia (2000 edition), i.e. L. japonica, L. hypoglauca,L. daystyla and L. confusa, other species such as L. similes and L. macranthoides have also been used on the same purpose in some local areas in China [2]. So it is an important issue to comprehensively evaluate the different sources of Flos Lonicerae, so as to ensure the clinical efficacy of this Chinese herbal drug.Chemical and pharmacological investigations on Flos Lonicerae resulted in discovering several kinds of bioactive components, i.e. chlorogenic acid and its analogues, flavonoids, iridoid glucosides and triterpenoid saponins [3]. Previously, chlorogenic acid has been used as the chemical marker for the quality evaluation of Flos Lonicerae,owing to its antipyretic and antibiotic property as well as its high content in the herb. But this compound is not a characteristic component of Flos Lonicerae, as it has also been used as the chemical marker for other Chinese herbal drugs such as Flos Chrysanthemi and so on[4-5]. Moreover, chlorogenic acid alone could not be responsible for the overall pharmacological activities of Flos Lonicerae[6].On the other hand, many studies revealed that triterpenoidal saponins of Flos Lonicerae possess protection effects on hepatic injury caused by Acetaminophen, Cd, and CCl4, and conspicuous depressant effects on swelling of ear croton oil [7-11]. Therefore, saponins should also be considered as one of the markers for quality control of Flos Lonicerae. Consequently, determinations of all types of components such as chlorogenic acid, flavonoids, iridoid glucosides and triterpenoidal saponins in Flos Lonicerae could be a better strategy for the comprehensive quality evaluation of Flos Lonicerae.Recently an HPLC-ELSD method has been established in our laboratory for qualitative and quantitative determination of iridoid glucosides in Flos Lonicerae [12]. But no method was reported for the determination of triterpenoidal saponins in Flos Lonicera. As a series studies on the comprehensive evaluation of Flos Lonicera, we report here, for the first time, the development of an HPLC-ELSD method for simultaneous determination of seven triterpenoidal saponins in the Chinese herbal drug Flos Lonicerae, i.e.macranthoidin B (1), macranthoidin A (2), dipsacoside B (3), hederagenin-28-O-β-D-glucopyranosyl(6→1)-O-β-D- glucopyranosyl ester (4), macranthoside B (5), macranthoside A (6), and hederagenin-3-O-α-L-arabinopyranosyl(2→1)-O-α-L-rhamnopyranoside (7) (Fig. 1).2. Experimental2.1. Samples, chemicals and reagentsFive samples of Lonicera species,L. japonica from Mi county, HeNan province (LJ1999-07), L. hypoglauca from Jiujang county, JiangXi province (LH2001-06), L. similes from Fei county, ShanDong province (LS2001-07), L. confuse from Xupu county, HuNan province (LC2001-07), and L. macranthoides from Longhu county, HuNan province (LM2000-06) respectively, were collected in China. All samples were authenticated by Dr. Ping Li, professor of department of Pharmacognosy, China Pharmaceutical University, Nanjing, China. The voucher specimens were deposited in the department of Pharmacognosy, China Pharmaceutical University, Nanjing, China. Seven saponin reference compounds: macranthoidin B (1), macranthoidin A (2), dipsacoside B (3), hederagenin-28-O-β-D-glucopyranosyl(6→1)-O-β-D- glucopyranosyl ester (4), macranthoside B (5), macranthoside A (6), and hederagenin-3-O-α-L-arabinopyranosyl(2→1)-O-α-L-rhamnopyranoside (7) were isolated previously from the dried buds of L. confusa by repeated silica gel, sephadex LH-20 and Rp-18 silica gel column chromatography, their structures were elucidated by comparison of their spectral data (UV, IR, MS, 1H- NMR and 13C-NMR) with references [13-15]. The purity of these saponins were determined to be more than 98% by normalization of the peak areas detected by HPLC with ELSD, and showed very stable in methanol solution.HPLC-grade acetonitrile from Merck (Darmstadt, Germany), the deionized water from Robust (Guangzhou, China), were purchased. The other solvents, purchased from Nanjing Chemical Factory (Nanjing, China) were of analytical grade.2.2. Apparatus and chromatographic conditionsAglient1100 series HPLC apparatus was used. Chromatography was carried out on an Aglient Zorbax SB-C18 column（250 4.6mm, 5.0µm）at a column temperature of 25℃.A Rheodyne 7125i sampling valve (Cotati, USA) equipped with a sample loop of 20µl was used for sample injection. The analog signal from Alltech ELSD 2000 (Alltech, Deerfield, IL, USA)was transmitted to a HP Chemstation for processing through an Agilent 35900E (Agilent Technologies, USA).The optimum resolution was obtained by using a linear gradient elution. The mobile phase was composed of acetonitrile(A) and water(B) which acidified with 0.5% acetic acid. The elution was operated from keeping 29%A for 10min, then gradually to 54%B from 10 to 25 min in linear gradient, and back to the isocratic elution of 54%B from 25 to 30 min.The drift tube temperature for ELSD was set at 106℃and the nitrogen flow-rate was of 2.6 l/min. The chromatographic peaks were identified by comparing their retention time with that of each reference compound tried under the same chromatographic conditions with a series of mobile phases. In addition, spiking samples with the reference compounds further confirmed the identities of the peaks.2.3. Calibration curvesMethanol stock solutions containing seven analytes were prepared and diluted to appropriate concentration for the construction of calibration curves. Six concentrationof the seven analytes’ solution were injected in triplicate, and then the calibration curves were constructed by plotting the peak areas versus the concentration of each analyte. The results were demonstrated in Table1.2.4. Limits of detection and quantificationMethanol stock solution containing seven reference compounds were diluted to a series of appropriate concentrations with methanol, and an aliquot of the diluted solutions were injected into HPLC for analysis.The limits of detection (LOD) and quantification (LOQ) under the present chromatographic conditions were determined at a signal-to-noise ratio (S/N) of 3 and 10, respectively. LOD and LOQ for each compound were shown in Table1.2.5. Precision and accuracyIntra- and inter-day variations were chosen to determine the precision of the developed assay. Approximate 2.0g of the pulverized samples of L. macranthoides were weighted, extracted and analyzed as described in 2.6 Sample preparation section. For intra-day variability test, the samples were analyzed in triplicate for three times within one day, while for inter-day variability test, the samples were examined in triplicate for consecutive three days. Variations were expressed by the relative standard deviations. The results were given in Table 2.Recovery test was used to evaluate the accuracy of this method. Accurate amounts of seven saponins were added to approximate 1.0g of L. macranthoides,and then extracted and analyzed as described in 2.6 Sample preparation section. The average recoveries were counted by the formula: recovery (%) = (amount found –original amount)/ amount spiked ×100%, and RSD (%) = (SD/mean) ×100%. The results were given in Table 3.2.6. Sample preparationSamples of Flos Lonicerae were dried at 50℃until constant weight. Approximate 2.0g of the pulverized samples, accurately weighed, was extracted with 60% ethanol in a flask for 4h. The ethanol was evaporated to dryness with a rotary evaporator. Residue was dissolved in water, followed by defatting with 60ml of petroleum ether for 2 times, and then the water solution was evaporated, residue was dissolved with methanol into a 25ml flask. One ml of the methanol solution was drawn and transferred to a 5ml flask, diluted to the mark with methanol. The resultant solution was at last filtrated through a 0.45µm syringe filter (Type Millex-HA, Millipore, USA) and 20µl of the filtrate was injected to HPLC system. The contents of the analytes were determined from the corresponding calibration curves.3. Results and discussionsThe temperature of drift tube and the gas flow-rate are two most important adjustable parameters for ELSD, they play a prominent role to an analyte response. In ourprevious work [12], the temperature of drift tube was optimized at 90°C for the determination of iridoids. As the polarity of saponins are higher than that of iridoids, more water was used in the mobile phase for the separation of saponins, therefore the temperature for saponins determination was optimized systematically from 95°C to 110°C, the flow-rate from 2.2 to 3.0 l/min. Dipsacoside B was selected as the testing saponin for optimizing ELSD conditions, as it was contained in all samples. Eventually, the drift tube temperature of 106℃and a gas flow of 2.6 l/min were optimized to detect the analytes. And these two exact experimental parameters should be strictly controlled in the analytical procedure [16].All calibration curves showed good linear regression (r2 0.9922) within test ranges. Validation studies of this method proved that this assay has good reproducibility. As shown in Table 2, the overall intra- and inter-day variations are less than 6% for all seven analytes. As demonstrated in Table 3, the developed analytical method has good accuracy with the overall recovery of high than 96% for the analytes concerned. The limit of detection (S/N=3) and the limit of quantification (S/N=10) are less than 0.26μg and 0.88μg respectively (Table1), indicating that this HPLC-ELSD method is precise, accurate and se nsitive enough for the quantitative evaluation of major non- chromaphoric saponins in Flos Lonicerae.It has been reported that there are two major types of saponins in Flos Lonicerae, i.e. saponins with hederagenin as aglycone and saponins with oleanolic acid as the aglycone [17]. But hederagenin type saponins of the herb were reported to have distinct activities of liver protection and anti-inflammatory [7-11]. So we adoptedseven hederagenin type saponins as representative markers to establish a quality control method.The newly established HPLC-ELSD method was applied to analyze seven analytes in five plant sources of Flos Lonicerae, i.e. L. japonica,L. hypoglauca,L. confusa,L. similes and L. macranthoides(Table 4). It was found that there were remarkable differences of seven saponins contents between different plant sources of Flos Lonicerae. All seven saponins analyzed could be detected in L. confusa and L. hypoglauca, while only dipsacoside B was detected in L. japonica. Among all seven saponins interested, only dipsacoside B was found in all five plant species of Flos Lonicerae analyzed, and this compound was determined as the major saponin with content of 53.7 mg/g in L. hypoglauca. On the other hand, macranthoidin B was found to be the major saponin with the content higher than 41.0mg/g in L. macranthoides,L. confusa, and L. similis, while the contents of other analytes were much lower.In our previous study [12], overall HPLC profiles of iridoid glucosides was used to qualitatively and quantitatively distinguish different origins of Flos Lonicerae. As shown in Fig.2, the chromatogram profiles of L. confusa, L. japonica and L. similes seem to be similar, resulting in the difficulty of clarifying the origins of Flos Lonicerae solely by HPLC profiles of saponins, in addition to the clear difference of the HPLC profiles of saponins from L. macranthoides and L. hypoglauca.Therefore, in addition to the conventional morphological and histological identification methods, the contents and the HPLC profiles of saponins and iridoids could also be used as accessory chemical evidence toclarify the botanical origin and comprehensive quality evaluation of Flos Lonicerae.4. ConclusionsThis is the first report on validation of an analytical method for qualification and quantification of saponins in Flos Lonicerae. This newly established HPLC-ELSD method can be used to simultaneously quantify seven saponins, i.e. macranthoidin B, macranthoidin A, dipsacoside B, hederagenin-28-O-β-D-glucopyranosyl(6→1)-O-β-D- glucopyranosyl ester, macranthoside B, macranthoside A, and hederagenin-3-O-α-L-arabinopyranosyl(2→1)-O-α-L-rhamnopyranoside in Flos Lonicerae. Together with the HPLC profiles of iridoids, the HPLC-ELSD profiles of saponins could also be used as an accessory chemical evidence to clarify the botanical origin and comprehensive quality evaluation of Flos Lonicerae.AcknowledgementsThis project is financially supported by Fund for Distinguished Chinese Young Scholars of the National Science Foundation of China (30325046) and the National High Tech Program（2003AA2Z2010）.[1]Ministry of Public Health of the People’s Republic of China, Pharmacopoeia ofthe People’s Republic of China, V ol.1, 2000, p. 177.[2]W. Shi, R.B. Shi, Y.R. Lu, Chin. Pharm. J., 34(1999) 724.[3]J.B. Xing, P. Li, D.L. Wen, Chin. Med. Mater., 26(2001) 457.[4]Y.Q. Zhang, L.C. Xu, L.P. Wang, J. Chin. Med. Mater., 21(1996) 204.[5] D. Zhang, Z.W. Li, Y. Jiang, J. Pharm. Anal., 16(1996) 83.[6]T.Z. Wang, Y.M. Li, Huaxiyaoxue Zazhi, 15(2000) 292.[7]J.ZH. Shi, G.T. Liu. Acta Pharm. Sin., 30(1995) 311.[8]Y. P. Liu, J. Liu, X.SH. Jia, et al. Acta Pharmacol. Sin., 13 (1992) 209.[9]Y. P. Liu, J. Liu, X.SH. Jia, et al. Acta Pharmacol. Sin., 13 (1992) 213.[10]J.ZH. Shi, L. Wan, X.F. Chen.ZhongYao YaoLi Yu LinChuang, 6 (1990) 33.[11]J. Liu, L. Xia, X.F. Chen. Acta Pharmacol. Sin., 9 (1988) 395[12]H.J. Li, P. Li, W.C. Ye, J. Chromatogr. A 1008(2003) 167-72.[13]Q. Mao, D. Cao, X.SH. Jia. Acta Pharm. Sin., 28(1993) 273.[14]H. Kizu, S. Hirabayashi, M. Suzuki, et al. Chem. Pharm. Bull., 33(1985) 3473.[15]S. Saito, S. Sumita, N. Tamura, et al. Chem Pharm Bull., 38(1990) 411.[16]Alltech ELSD 2000 Operating Manual, Alltech, 2001, p. 16. In Chinese.[17]J.B. Xing, P. Li, Chin. Med. Mater., 22(1999) 366.Fig. 1 Chemical structures of seven saponins from Lonicera confusa macranthoidin B (1), macranthoidin A (2), dipsacoside B (3), hederagenin-28-O-β-D-glucopyranosyl(6→1)-O-β-D- glucopyranosyl ester (4), macranthoside B (5), macranthoside A (6), and hederagenin-3-O-α-L-arabinopyranosyl(2→1)-O-α-L-rhamnopyranoside (7)Fig. 2Representative HPLC chromatograms of mixed standards and methanol extracts of Flos Lonicerae.Column: Agilent Zorbax SB-C18 column（250 4.6mm, 5.0µm）, temperature of 25℃; Detector: ELSD, drift tube temperature 106℃, nitrogen flow-rate 2.6 l/min.A: Mixed standards, B: L. confusa, C: L. japonica, D: L. macranthoides, E: L. hypoglauca, F: L. similes.Table 1 Calibration curves for seven saponinsAnalytes Calibration curve ar2Test range(μg)LOD(μg)LOQ(μg)1 y=6711.9x－377.6 0.9940 0.56–22.01 0.26 0.882 y=7812.6x－411.9 0.9922 0.54–21.63 0.26 0.843 y=6798.5x－299.0 0.9958 0.46–18.42 0.22 0.724 y=12805x－487.9 0.9961 0.38–15.66 0.10 0.345 y=4143.8x－88.62 0.9989 0.42–16.82 0.18 0.246 y=3946.8x－94.4 0.9977 0.40–16.02 0.16 0.207 y=4287.8x－95.2 0.9982 0.42–16.46 0.12 0.22a y: Peak area; x: concentration (mg/ml)Table 2 Reproducibility of the assayAnalyteIntra-day variability Inter-day variability Content (mg/g) Mean RSD (%) Content (mg/g) Mean RSD (%)1 46.1646.2846.2246.22 0.1346.2245.3647.4226.33 2.232 5.385.385.165.31 2.405.285.345.045.22 3.043 4.374.304.184.28 2.244.284.464.024.255.204 nd1)-- -- nd -- --5 1.761.801.821.79 1.701.801.681.841.77 4.706 1.281.241.221.252.451.241.341.201.26 5.727 tr2)-- -- tr -- -- 1): not detected; 2): trace. RSD (%) = (SD/Mean) ×100%Table 3 Recovery of the seven analytesAnalyteOriginal(mg) Spiked(mg)Found(mg)Recovery(%)Mean(%)RSD(%)1 23.0823.1423.1119.7122.8628.1042.7346.1351.0199.7100.699.399.8 0.722.692.672.582.082.913.164.735.515.7698.197.6100.698.8 1.632.172.152.091.732.182.623.884.404.6598.8103.297.799.9 2.94nd1)1.011.050.980.981.101.0297.0104.8104.1102.0 4.250.880.900.910.700.871.081.561.752.0197.197.7101.898.9 2.660.640.620.610.450.610.751.081.211.3397.796.796.096.8 0.97tr2)1.021.101.081.031.111.07100.9102.799.1100.9 1.81): not detected; 2): trace.a Recovery (%) = (Amount found –Original amount)/ Amount spiked ×100%, RSD (%) = (SD/Mean) ×100%Table 4 Contents of seven saponins in Lonicera spp.Content (mg/g)1 2 3 4 5 6 7 L. confusa45.65±0.32 5.13±0.08 4.45±0.11tr1) 2.04±0.04tr 1.81±0.03 L. japonica nd2)nd 3.44±0.09nd nd nd nd L. macranthoides46.22±0.06 5.31±0.13 4.28±0.10 tr 1.79±0.03 1.25±0.03 tr L. hypoglauca11.17±0.07 nq3)53.78±1.18nd 1.72±0.02 2.23±0.06 2.52±0.04 L. similes41.22±0.25 4.57±0.07 3.79±0.09nd 1.75±0.02tr nd 1): trace; 2): not detected.. 3) not quantified owing to the suspicious purity of the peak.。
一种西格列汀中亚硝胺类杂质的制备方法
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一种西格列汀中亚硝胺类杂质的制备方法1.背景介绍我准备先从主题的背景介绍开始，引入读者对这一主题的基本了解。
西格列汀是一种常用的药物，但其中亚硝胺类杂质可能对人体健康造成潜在威胁。
制备一种方法来有效去除或限制亚硝胺类杂质的存在至关重要。
2.西格列汀中亚硝胺类杂质的危害和影响在文章的第二部分，我将详细探讨亚硝胺类杂质对西格列汀药物品质和患者健康的潜在危害和影响。
这一部分将会涉及全面的研究成果和数据，以确保读者充分理解这一问题的严重性。
3.现有解决方式的不足为了更深入地探究这一问题，我准备详细分析当前常用的制备方法，揭示它们在去除亚硝胺类杂质方面存在的不足和局限性。
这一部分将引导读者理解为什么需要一种新的、更有效的制备方法。
4.新制备方法的原理和步骤紧我将着重介绍这种新制备方法的原理和具体操作步骤。
这部分将包括详细的化学反应方程式和实验操作流程，确保读者对该方法的操作和原理有清晰的理解。
5.新方法的优势和潜在应用价值接下来，我打算通过对这种新制备方法的优势和潜在应用价值进行分析，向读者展示其在应对亚硝胺类杂质问题上的独特地位和重要意义。
这一部分将包括实验数据和结果的引用，以提供更具说服力的论据。
6.个人观点和总结我将共享我个人对这一主题的观点和理解，并通过全文的回顾和总结来确保读者全面、深刻并灵活地理解这一主题。
以上每个部分都将详细展开，以确保文章的深度和广度兼具。
希望这篇文章能为您提供有价值的信息，并满足您的要求。
我将竭尽全力撰写出一篇高质量的文章，以拓宽您对这一主题的认识和理解。
背景介绍：西格列汀是一种常用的口服降糖药物，用于治疗2型糖尿病。
然而，西格列汀中存在的亚硝胺类杂质可能对人体健康造成潜在威胁。
亚硝胺类化合物是一类致癌的化学物质，它们可能会对身体内的DNA造成损害，增加患癌症的风险。
Cisplatin_SDS_MedChemExpress
Inhibitors, Agonists, Screening LibrariesSafety Data Sheet Revision Date:Jul.-12-2017Print Date:Jul.-12-20171. PRODUCT AND COMPANY IDENTIFICATION1.1 Product identifierProduct name :CisplatinCatalog No. :HY-17394CAS No. :15663-27-11.2 Relevant identified uses of the substance or mixture and uses advised againstIdentified uses :Laboratory chemicals, manufacture of substances.1.3 Details of the supplier of the safety data sheetCompany:MedChemExpress USATel:609-228-6898Fax:609-228-5909E-mail:sales@1.4 Emergency telephone numberEmergency Phone #:609-228-68982. HAZARDS IDENTIFICATION2.1 Classification of the substance or mixtureGHS Classification in accordance with 29 CFR 1910 (OSHA HCS)Acute toxicity, Oral (Category 2), H300Serious eye damage (Category 1), H318Carcinogenicity (Category 1B), H3502.2 GHS Label elements, including precautionary statementsPictogramSignal word DangerHazard statement(s)H300 Fatal if swallowed.H318 Causes serious eye damage.H350 May cause cancer.Precautionary statement(s)P201 Obtain special instructions before use.P202 Do not handle until all safety precautions have been read and understood.P264 Wash skin thoroughly after handling.P270 Do not eat, drink or smoke when using this product.P280 Wear protective gloves/ eye protection/ face protection.P301 + P310 IF SWALLOWED: Immediately call a POISON CENTER or doctor/physician.P305 + P351 + P338 IF IN EYES: Rinse cautiously with water for several minutes. Remove contactlenses, if present and easy to do. Continue rinsing.P310 Immediately call a POISON CENTER or doctor/ physician.H300 Fatal if swallowed.H318 Causes serious eye damage.H350 May cause cancer. P321 Specific treatment (see supplemental first aid instructions on this label).P330 Rinse mouth.P405 Store locked up.P501 Dispose of contents/ container to an approved waste disposal plant.2.3 Other hazardsNone.3. COMPOSITION/INFORMATION ON INGREDIENTS3.1 SubstancesSynonyms:CDDP; cis–DiaminodichloroplatinumFormula:Cl2H6N2PtMolecular Weight:300.05CAS No. :15663-27-14. FIRST AID MEASURES4.1 Description of first aid measuresEye contactRemove any contact lenses, locate eye-wash station, and flush eyes immediately with large amounts of water. Separate eyelids with fingers to ensure adequate flushing. Promptly call a physician.Skin contactRinse skin thoroughly with large amounts of water. Remove contaminated clothing and shoes and call a physician.InhalationImmediately relocate self or casualty to fresh air. If breathing is difficult, give cardiopulmonary resuscitation (CPR). Avoid mouth-to-mouth resuscitation.IngestionWash out mouth with water; Do NOT induce vomiting; call a physician.4.2 Most important symptoms and effects, both acute and delayedThe most important known symptoms and effects are described in the labelling (see section 2.2).4.3 Indication of any immediate medical attention and special treatment neededTreat symptomatically.5. FIRE FIGHTING MEASURES5.1 Extinguishing mediaSuitable extinguishing mediaUse water spray, dry chemical, foam, and carbon dioxide fire extinguisher.5.2 Special hazards arising from the substance or mixtureDuring combustion, may emit irritant fumes.5.3 Advice for firefightersWear self-contained breathing apparatus and protective clothing.6. ACCIDENTAL RELEASE MEASURES6.1 Personal precautions, protective equipment and emergency proceduresUse full personal protective equipment. Avoid breathing vapors, mist, dust or gas. Ensure adequate ventilation. Evacuate personnel to safe areas.Refer to protective measures listed in sections 8.6.2 Environmental precautionsTry to prevent further leakage or spillage. Keep the product away from drains or water courses.6.3 Methods and materials for containment and cleaning upAbsorb solutions with finely-powdered liquid-binding material (diatomite, universal binders); Decontaminate surfaces and equipment by scrubbing with alcohol; Dispose of contaminated material according to Section 13.7. HANDLING AND STORAGE7.1 Precautions for safe handlingAvoid inhalation, contact with eyes and skin. Avoid dust and aerosol formation. Use only in areas with appropriate exhaust ventilation.7.2 Conditions for safe storage, including any incompatibilitiesKeep container tightly sealed in cool, well-ventilated area. Keep away from direct sunlight and sources of ignition.Recommended storage temperature:Powder-20°C 3 years4°C 2 yearsIn solvent-80°C 6 months-20°C 1 monthShipping at room temperature if less than 2 weeks.7.3 Specific end use(s)No data available.8. EXPOSURE CONTROLS/PERSONAL PROTECTION8.1 Control parametersComponents with workplace control parametersThis product contains no substances with occupational exposure limit values.8.2 Exposure controlsEngineering controlsEnsure adequate ventilation. Provide accessible safety shower and eye wash station.Personal protective equipmentEye protection Safety goggles with side-shields.Hand protection Protective gloves.Skin and body protection Impervious clothing.Respiratory protection Suitable respirator.Environmental exposure controls Keep the product away from drains, water courses or the soil. Cleanspillages in a safe way as soon as possible.9. PHYSICAL AND CHEMICAL PROPERTIES9.1 Information on basic physical and chemical propertiesAppearance Light yellow to yellow (Solid)Odor No data availableOdor threshold No data availablepH No data availableMelting/freezing point No data availableBoiling point/range No data available Flash point No data available Evaporation rate No data available Flammability (solid, gas)No data available Upper/lower flammability or explosive limits No data available Vapor pressure No data available Vapor density No data available Relative density No data available Water Solubility No data available Partition coefficient No data available Auto-ignition temperature No data available Decomposition temperature No data available Viscosity No data available Explosive properties No data available Oxidizing properties No data available 9.2 Other safety informationNo data available.10. STABILITY AND REACTIVITY10.1 ReactivityNo data available.10.2 Chemical stabilityStable under recommended storage conditions.10.3 Possibility of hazardous reactionsNo data available.10.4 Conditions to avoidNo data available.10.5 Incompatible materialsStrong acids/alkalis, strong oxidising/reducing agents.10.6 Hazardous decomposition productsUnder fire conditions, may decompose and emit toxic fumes.Other decomposition products - no data available.11.TOXICOLOGICAL INFORMATION11.1 Information on toxicological effectsAcute toxicityClassified based on available data. For more details, see section 2Skin corrosion/irritationClassified based on available data. For more details, see section 2Serious eye damage/irritationClassified based on available data. For more details, see section 2Respiratory or skin sensitizationClassified based on available data. For more details, see section 2Germ cell mutagenicityClassified based on available data. For more details, see section 2CarcinogenicityIARC: No component of this product present at a level equal to or greater than 0.1% is identified as probable, possible or confirmed human carcinogen by IARC.ACGIH: No component of this product present at a level equal to or greater than 0.1% is identified as a potential or confirmed carcinogen by ACGIH.NTP: No component of this product present at a level equal to or greater than 0.1% is identified as a anticipated or confirmed carcinogen by NTP.OSHA: No component of this product present at a level equal to or greater than 0.1% is identified as a potential or confirmed carcinogen by OSHA.Reproductive toxicityClassified based on available data. For more details, see section 2Specific target organ toxicity - single exposureClassified based on available data. For more details, see section 2Specific target organ toxicity - repeated exposureClassified based on available data. For more details, see section 2Aspiration hazardClassified based on available data. For more details, see section 2Additional informationRTECS No.: TP2450000May cause liver irregularities.This information is based on our current knowledge. However the chemical, physical, and toxicological properties have not been completely investigated.12. ECOLOGICAL INFORMATION12.1 ToxicityNo data available.12.2 Persistence and degradabilityNo data available.12.3 Bioaccumlative potentialNo data available.12.4 Mobility in soilNo data available.12.5 Results of PBT and vPvB assessmentPBT/vPvB assessment unavailable as chemical safety assessment not required or not conducted.12.6 Other adverse effectsNo data available.13. DISPOSAL CONSIDERATIONS13.1 Waste treatment methodsProductDispose substance in accordance with prevailing country, federal, state and local regulations.Contaminated packagingConduct recycling or disposal in accordance with prevailing country, federal, state and local regulations.14. TRANSPORT INFORMATIONDOT (US)This substance is considered to be non-hazardous for transport.IMDGThis substance is considered to be non-hazardous for transport.IATAThis substance is considered to be non-hazardous for transport.15. REGULATORY INFORMATIONAcute Health Hazard, Chronic Health Hazard.16. OTHER INFORMATIONCopyright 2017 MedChemExpress. The above information is correct to the best of our present knowledge but does not purport to be all inclusive and should be used only as a guide. The product is for research use only and for experienced personnel. It must only be handled by suitably qualified experienced scientists in appropriately equipped and authorized facilities. The burden of safe use of this material rests entirely with the user. MedChemExpress disclaims all liability for any damage resulting from handling or from contact with this product.Caution: Product has not been fully validated for medical applications. For research use only.Tel: 609-228-6898 Fax: 609-228-5909 E-mail: tech@Address: 1 Deer Park Dr, Suite Q, Monmouth Junction, NJ 08852, USA。
支气管肺泡灌洗液中生物标志物在特发性肺纤维化中的研究进展
-D 浓 度 高 于 结 节 病
断可能需要多个标志物。
骨膜蛋白是一种细胞外基质细 胞 蛋 白, 属
结节 病 组 [(
7 05±12 79)pg/g] 及 对 照 组 [(
1 84±
(
S100A9/MRP14) 水平升高,可为 IPF 的诊断提供依据。
黏蛋白是糖蛋白的一种,是由分泌 细 胞 分 泌
外表面 表 达 的 糖 蛋 白, 目 前 被 认 为 是 可 与 IPF 表 现 相 同 或 类 似。 急 性
IPF 诊断性生 物 标 志 物, 其 确 切 的 功 能 尚 不 清 楚。 作 为 一
诊断 IPF、监测 IPF 进 展、 判 断 IPF 预 后 的 生 物 标 志 物 受
程中,正常健康肺组 织 被 明 显 破 坏 的 肺 泡 结 构 和 改 变 的 细
胞外基质所取代。这 些 变 化 导 致 肺 气 体 交 换 中 断, 顺 应 性
降低,最终导致 呼 吸 衰 竭 和 死 亡 [2]。IPF 的 5 年 生 存 率 在
20%~40% 之间,死亡 率 高 于 结 肠 癌、 多 发 性 骨 髓 瘤 和 膀
6
和 SP
-D 相比,单 体 骨 膜 蛋 白 对 IPF 的 识 别 能 力 最 强。 传
广泛表 达, 分 别 为 MUC5AC 和 MUC5B, MUC5AC 主 要
在 一项对IPF 患者 BALF 的定量蛋白质组学的研究中发现,
气道上皮细胞在中性 粒 细 胞 弹 性 蛋 白 酶 和 活 化 的 嗜 酸 粒 细
和其他高危疾病 (特 应 性 皮 炎、 系 统 性 硬 皮 病 和 哮 喘 ) 患
由近端气 道 产 生, 而 MUC5B 主 要 表 达 于 远 端 呼 吸 道 [19]。
基于GC-MS与网络药理学的青皮挥发油防治阿尔茨海默症的活性成分及作用机制研究
基于GC-MS与网络药理学的青皮挥发油防治阿尔茨海默症的活性成分及作用机制研究作者：王腾华罗颖懿王驭辰任之尧唐建新李咏梅方翼吴波来源：《中国药房》2020年第17期摘要目的：预测青皮挥发油防治阿尔茨海默病（AD）的主要活性成分和潜在作用靶点。
方法：采用气质联用技术（GC-MS）分析青皮挥发油化学成分，并借助NIST 11.L数据库和人工数据解析进行成分的结构鉴定。
借助中药系统药理学分析平台（TCMSP）、PharmMapper数据库等预测青皮挥发油活性成分及其对应靶点，借助GeneCards数据库、人类孟德尔遗传数据库等挖掘AD相关靶点;利用Venny 2.1.0软件映射以获取青皮挥发油防治AD的直接靶点;借助STRING数据库和Cytoscape 7.2.1软件挖掘核心节点，利用Venny 2.1.0软件映射并去重后获取青皮挥发油防治AD的间接靶点;借助DAVID 6.7數据库对上述直接和间接靶点（即作用靶点）进行基因本体（GO）功能富集和KEGG通路富集分析;采用Cytoscape 7.2.1软件，以节点度值、介数中心度、紧密中心度为指标，对青皮挥发油“活性成分-作用靶点”网络进行拓扑学分析，挖掘关键成分和关键靶点。
结果与结论：GC-MS法共分离并鉴定出青皮挥发油化学成分40个，均为活性成分，包括右旋柠檬烯、γ-萜品烯等。
共挖掘出活性成分对应靶点151个、AD相关靶点1 291个，其中直接靶点48个、间接靶点41个。
上述89个作用靶点主要富集于细胞分数、轴突、胞浆等细胞组分，细胞内信号级联、对有机物的反应等生物过程，蛋白激酶活性、胺受体活性等分子功能，以及癌症通路、钙信号通路、神经营养素信号通路等信号通路（P关键词青皮;挥发油;气质联用技术;网络药理学;阿尔茨海默病;机制ABSTRACT OBJECTIVE： To predict the active components and potential target of volatile oil of Citri reticulatae preventing and treating Alzheimer’s disease （AD）. METHODS： The volatile oil of C. reticulatae was determined by GC-MS， and identified according to NIST 11.L database and manual data analysis. The active components and targets of volatile oil of C. reticulatae were predicted through TCMSP and PharmMapper database. The related targets of AD were obtained by using GeneCards and OMIM databases. Venny 2.1.0 software mapping was used to obtain the direct targets of volatile oil of C. reticulatae against AD. Core nodes were mined with STRING database andCytoscape 7.2.1 software， and the indirect targets of volatile oil of C. reticulatae against AD were obtained by mapping and duplication coith Venny 2.1.0 software. With the help of DAVID 6.7 database， the above direct and indirect targets （i.e. action targets） were used for gene ontology （GO） function enrichment analysis and KEGG pathway enrichment analysis. Using Cytoscape7.2.1 software，topology analysis was conducted for the network of “active components-acting targets” of volatile oil of C. reticulatae， with node degree value， betweenness centrality and closeness centrality as indexes， then key components and key targets were mined. RESULTS & CONCLUSIONS： A total of 40 chemical components in volatile oil were identified by GC-MS， all of them were active components， including D-limonene，γ-terpinene， etc. A total of 151 active components-corresponding targets and 1 291 AD-related targets were mined， including 48 direct targets and 41 indirect targets. The above 89 targets were mainly concentrated in cell fraction，axon， cytosol and other cell components; intracellular signaling cascade， response to organic substance and other biological processes; protein kinase activity and amine receptor activity and other molecular functions; as well as cancer pathway， calcium signaling pathway and neurotrophin signaling pathway （PKEYWORDS Citri reticulatae; Volatile oil; GC-MS; Network pharmacology; Alzheimer’s disease; Mechanism青皮为芸香科植物橘（Citrus reticulata Blanco）及其栽培变种的干燥幼果或未成熟果实的果皮。
基质效应在生物样品质谱分析中的优化措施研究
基质效应在生物样品质谱分析中的优化措施研究吴文静【摘要】高效液相色谱-质谱联用法（LC - MS /MS ）由于其高灵敏度和高选择性现阶段被广泛应用于食品检测、环境评估等方面的样品定量分析.然而,由于实际样品特别是复杂样品分析中基质效应的存在,样品分析进程以及检测结果的特异性、灵敏度和准确度都会受到影响.本文立足于实际的生物样品质谱分析,阐述了基质效应的产生原因、检测及评定方法,其优化措施包括四个方面,即样品前处理的优化、色谱条件的优化、质谱条件的优化以及同位素内标的选择.【期刊名称】《信阳农林学院学报》【年(卷),期】2017(027)004【总页数】5页(P115-118)【关键词】高效液相色谱一质谱联用基质效应生物样品分析【作者】吴文静【作者单位】安徽公安职业学院公安科学技术系,安徽合肥230031;【正文语种】中文【中图分类】O657.63高效液相色谱－质谱联用法（液相质谱，HPLC－MS／MS）是一种高灵敏度和高选择性的样品定量分析方法，由于其高效样品的选择性和准确的测定能力而被广泛推广应用于食品相关检测、环境风险评估、农药残留分析、药物组分以及代谢研究中［1－2］。
近几年，随着液质技术的快速发展，与检测相关的基质效应问题也开始被广泛关注。
基质效应作为质谱检测中存在的必然问题，对样品检测、分析方法和结果的特异性、灵敏度和准确度都有显著影响［3］。
目前，国外的学者已经开展了大量的与基质效应相关的工作和研究，但国内相关的研究还未能构成完整的研究体系。
本文结合国内外相关文献，对液质检测过程中基质效应的产生原因、相关作用以及目前常规的检测方法和消除或降低基质干扰的途径等问题进行阐述。
1 基质效应产生机制及影响基质效应指的是在样品检测过程中，除待测组分以外的其它物质对待测组分的分析进程产生的干扰，并影响检测结果的灵敏度和准确性。
基质效应的产生主要是源于样品中的待测组分与基质成分在离子化过程中的竞争。
液相色谱-串联质谱法检测血液中的美西律
液相色谱-串联质谱法检测血液中的美西律严慧;向平;卜俊;沈敏【摘要】目的建立测定血液中美西律(mexiletine)的液相色谱-串联质谱联用法(LC-MS/MS).方法采用简便的乙腈蛋白沉淀法对血液进行预处理,应用Allure PAP Propel液相柱分离,用电喷雾正离子模式离子化,多反应监测模式对美西律进行分析.结果美西律与内标纳洛酮分离良好,在0.02～10.00μg/mL内线性关系良好,相关系数为0.9999,回归方程为y=0.028 3x-0.015 1,日内与日间精密度的RSD均小于15%,最低检测限为0.01μg/ml.结论建立的L.C.-MS/MS方法简单、灵敏、可靠,可同时适用于美西律临床药物监测和法医毒物分析的需要.【期刊名称】《法医学杂志》【年(卷),期】2007(023)006【总页数】3页(P441-443)【关键词】LC-MS/MS;抗心律失常药;美西律;血液【作者】严慧;向平;卜俊;沈敏【作者单位】司法部司法鉴定科学技术研究所,上海,200063;复旦大学上海医学院法医学系,上海,200032;司法部司法鉴定科学技术研究所,上海,200063;司法部司法鉴定科学技术研究所,上海,200063;司法部司法鉴定科学技术研究所,上海,200063【正文语种】中文【中图分类】DF795.4美西律（Mexiletine）是常用的钠通道阻滞类抗心律失常药，能阻滞心肌细胞膜、快钠通道，对室性心律失常的疗效较好[1]。
美西律的有效血药质量浓度范围为0．7～2μg/mL[2],中毒血药质量浓度与有效血药质量浓度相近,为2μg/mL以上，因此监测其血药质量浓度极为必要。
美西律服用剂量过大时可出现心律减慢、血压下降、房室传导阻滞和视力模糊等症状，严重者可致呼吸抑制死亡。
有关美西律中毒的案例时有发生[3-5]。
目前国内外对美西律的测定方法主要有气相色谱-质谱联用法（GC-MS）[2-3]、高效液相色谱法(HPLC)[6]、毛细管电泳法(CE)[7-8]、液相色谱-串联质谱联用法(LCMS/MS)[9]等。