A simple, sensitive and accurate method based on high performance liquid chromato- graphy （HPLC） with diode array detector （DAD） was developed and validated for systematic quality evaluation of one type of traditi...A simple, sensitive and accurate method based on high performance liquid chromato- graphy （HPLC） with diode array detector （DAD） was developed and validated for systematic quality evaluation of one type of traditional Chinese medicine preparations named Xinkeshu （XKS） tablet. In this study, the chromatographic fingerprints of XKS tablet were developed first, 23 peaks were selected as the common peaks to evaluate the similarities among different batches of XKS samples, which were manufactured in a long time span of three years. Additionally, simultaneous quantification of six markers in XKS tablet, including Danshensu, Protocatechuic aldehyde, Puerarin, Daidzin, Salvianolic acid B and Daidzein, was performed. The validation results showed that the developed method was specific, accurate, precise and robust. The preliminary explanation on why a close similarity between fingerprints did not exactly mean similar contents of chemical components in samples was given. The contribution of each chromatographic peak to similarity was also evaluated. The developed method offers an efficient, reliable and practical approach for systematic quality evaluation of XKS tablet.展开更多
A simple, precise, and rapid high-performance liquid chromatographic method was developed and validated for the simultaneous determination of vitexin-2＂-O-glucoside, vitexin-2＂-O-rhamnoside, rutin, vitexin, and hype...A simple, precise, and rapid high-performance liquid chromatographic method was developed and validated for the simultaneous determination of vitexin-2＂-O-glucoside, vitexin-2＂-O-rhamnoside, rutin, vitexin, and hyperoside. The HPLC separation was performed using a Shim-pack VP-ODS C18 column （250 mm ~ 4.6 mm i.d., 5 ~tm） with the isocratic mobile phase consisting of tetrahydrofuran/ acetonitrile/0.05% phosphoric acid solution （20：3：77, v/v/v）, and the flow rate was set at 1.0 mL/min. UV detection was carried out at a wavelength of 360 nrn and the whole analysis took 25 min. The method was linear in the range of 4.12-206.00 μg/mL for vitexin-2＂-O-glucoside, 4.05-202.50 μg/mL for vitexin-2＂-O- rhanmoside, 1.64-82.00 pμg/mL for rutin, 1.74-87.00 gg/mL for vitexin, and 1.41-70.60 p.g/mL for hyperoside with the correlation coefficient for each analyte more than 0.998. The limit of detection （LOD） and limit of quantitation （LOQ） were 0.6 and 2 ng for vitexin-2＂-O-glucoside, 0.6 and 2 ng for vitexin-2＂-O-rhamnoside, 0.3 and 1 ng for rutin, 1 and 3 ng for vitexin, and 0.5 and 2 ng for hyperoside, respectively. Intra- and inter-day precision and accuracy （RSD） were less than 3%. The developed HPLC method was successfully applied to the analysis of five flavonoids in hawthorn leaves, hawthorn fruits, and the preparations containing hawthorn leaves or fruits.展开更多
With the expansion of herbal medicine （HM） market, the issue on how to apply up-to- date analytical tools on qualitative analysis of HMs to assure their quality, safety and efficacy has been arousing great attention...With the expansion of herbal medicine （HM） market, the issue on how to apply up-to- date analytical tools on qualitative analysis of HMs to assure their quality, safety and efficacy has been arousing great attention. Due to its inherent characteristics of accurate mass measurements and multiple stages analysis, the integrated strategy of liquid chromatography （LC） coupled with time-of-flight mass spectrometry （TOF-MS） and ion trap mass spectrometry （IT-MS） is well-suited to be performed as qualitative analysis tool in this field. The purpose of this review is to provide an overview on the potential of this integrated strategy, including the review of general features of LC-IT-MS and LC-TOF-MS, the advantages of their combination, the common procedures for structure elucidation, the potential of LC-hybrid-IT-TOF/MS and also the summary and discussion of the applications of the integrated strategy for HM qualitative analysis （2006-2011）. The advantages and future developments of LC coupled with IT and TOF-MS are highlighted.展开更多
Euphorbia lathyris （Caper spurge） is a toxic and potent Chinese materia medica （T/PCMM）. This study sought a method for identifying five diterpenoids （Euphorbia factors LI-L3, L7a, and Ls） with the spectra of UV...Euphorbia lathyris （Caper spurge） is a toxic and potent Chinese materia medica （T/PCMM）. This study sought a method for identifying five diterpenoids （Euphorbia factors LI-L3, L7a, and Ls） with the spectra of UV and mass, quantifying three diterpenoids L1, L2, and L8 in crude extracts of unprocessed and processed E. lathyris seeds by liquid chromatography/ electrospray ionization mass spectrometry （LC-ESI-MS）. The analysis was achieved on an Agilent Eclipse XDB-C18 column （4.6 mm× 150mm i.d., 5 μm） with an isocratic elution with a mobile phase consisting of water and acetonitrile at a flow rate of 0.25 mL/min at column temperature of 30 ℃ and UV detection was set at 272 nm. An ESI source was used with a positive ionization mode. The calibration curve was linear in the ranges of 9.9-79 μg/mL for Euphorbia factor Lb 3.8-30.5μg/mL for Euphorbia factor L2, and 1.0-20.6 μg/mL for Euphorbia factor LB. The average recoveries （n=6） of three diterpenoids were 98.39%, 91.10% and 96.94%, respectively, with RSD of 2.5%, 2.4% and 2.1%, respectively. The contents of the three diterpenoids in processed E. lathyris seeds were 3.435, 1.367 and 0.286 mg/g, respectively, which decreased more sharply than those in unprocessed E. lathyris seeds which were 4.915, 1.944 and 0.425 mg/g, respectively. The method is simple, accurate, reliable and reproducible, and it can be applied to control the quality of unprocessed and processed E. lathyris seeds.展开更多
目的:比较试验和参比制剂2.5%复方利多卡因乳膏透皮作用的一致性。方法:以大鼠和巴马香猪的皮肤作为透皮渗透的材料,选用立式改良Franz扩散池测定复方利多卡因乳膏的渗透吸收规律,以高效液相色谱法分别测定接收液中药物的吸收总量和猪...目的:比较试验和参比制剂2.5%复方利多卡因乳膏透皮作用的一致性。方法:以大鼠和巴马香猪的皮肤作为透皮渗透的材料,选用立式改良Franz扩散池测定复方利多卡因乳膏的渗透吸收规律,以高效液相色谱法分别测定接收液中药物的吸收总量和猪皮中药物的滞留量随时间的变化关系。结果:复方利多卡因乳膏试验与参比制剂在鼠皮及巴马香猪皮这两种不同透皮材料中5 h利多卡因的单位面积累积渗透量分别为(0.380±0.019)和(0.351±0.017)mg·cm^(-2),(0.228±0.012)和(0.217±0.023)mg·cm^(-2);丙胺卡因的单位面积累积渗透量分别为(0.422±0.022)和(0.382±0.029)mg·cm^(-2),(0.263±0.015)和(0.238±0.008)mg·cm^(-2);试验制剂与参比制剂在巴马香猪皮中5h的利多卡因,丙胺卡因的皮内滞留量分别为(2.021±0.094)和(1.999±0.118)mg·cm^(-2),(2.240±0.115)和(2.208±0.053)mg·cm^(-2);试验和参比制剂的体外释放比较的结果均符合FDA(U.S.Food and Drug Administration)和欧盟的指导原则。结论:2.5%复方利多卡因乳膏试验与参比制剂的透皮渗透程度和速率均符合外用制剂的一致性要求,且在猪皮内药物滞留特征相似。展开更多
基金supported by the Major Projects of Independent Innovation Achievements of Shandong Province(No. 2010ZDZX1A0406)partly by the Scientific and Technological Projects of Shandong Province (No. 2009GG10002081)+1 种基金Independent Innovation Foundation of Shandong University(No. 2010TS054)Shandong Province Natural Science Foundation, China (No. ZR2011HM080)
文摘A simple, sensitive and accurate method based on high performance liquid chromato- graphy （HPLC） with diode array detector （DAD） was developed and validated for systematic quality evaluation of one type of traditional Chinese medicine preparations named Xinkeshu （XKS） tablet. In this study, the chromatographic fingerprints of XKS tablet were developed first, 23 peaks were selected as the common peaks to evaluate the similarities among different batches of XKS samples, which were manufactured in a long time span of three years. Additionally, simultaneous quantification of six markers in XKS tablet, including Danshensu, Protocatechuic aldehyde, Puerarin, Daidzin, Salvianolic acid B and Daidzein, was performed. The validation results showed that the developed method was specific, accurate, precise and robust. The preliminary explanation on why a close similarity between fingerprints did not exactly mean similar contents of chemical components in samples was given. The contribution of each chromatographic peak to similarity was also evaluated. The developed method offers an efficient, reliable and practical approach for systematic quality evaluation of XKS tablet.
文摘A simple, precise, and rapid high-performance liquid chromatographic method was developed and validated for the simultaneous determination of vitexin-2＂-O-glucoside, vitexin-2＂-O-rhamnoside, rutin, vitexin, and hyperoside. The HPLC separation was performed using a Shim-pack VP-ODS C18 column （250 mm ~ 4.6 mm i.d., 5 ~tm） with the isocratic mobile phase consisting of tetrahydrofuran/ acetonitrile/0.05% phosphoric acid solution （20：3：77, v/v/v）, and the flow rate was set at 1.0 mL/min. UV detection was carried out at a wavelength of 360 nrn and the whole analysis took 25 min. The method was linear in the range of 4.12-206.00 μg/mL for vitexin-2＂-O-glucoside, 4.05-202.50 μg/mL for vitexin-2＂-O- rhanmoside, 1.64-82.00 pμg/mL for rutin, 1.74-87.00 gg/mL for vitexin, and 1.41-70.60 p.g/mL for hyperoside with the correlation coefficient for each analyte more than 0.998. The limit of detection （LOD） and limit of quantitation （LOQ） were 0.6 and 2 ng for vitexin-2＂-O-glucoside, 0.6 and 2 ng for vitexin-2＂-O-rhamnoside, 0.3 and 1 ng for rutin, 1 and 3 ng for vitexin, and 0.5 and 2 ng for hyperoside, respectively. Intra- and inter-day precision and accuracy （RSD） were less than 3%. The developed HPLC method was successfully applied to the analysis of five flavonoids in hawthorn leaves, hawthorn fruits, and the preparations containing hawthorn leaves or fruits.
文摘With the expansion of herbal medicine （HM） market, the issue on how to apply up-to- date analytical tools on qualitative analysis of HMs to assure their quality, safety and efficacy has been arousing great attention. Due to its inherent characteristics of accurate mass measurements and multiple stages analysis, the integrated strategy of liquid chromatography （LC） coupled with time-of-flight mass spectrometry （TOF-MS） and ion trap mass spectrometry （IT-MS） is well-suited to be performed as qualitative analysis tool in this field. The purpose of this review is to provide an overview on the potential of this integrated strategy, including the review of general features of LC-IT-MS and LC-TOF-MS, the advantages of their combination, the common procedures for structure elucidation, the potential of LC-hybrid-IT-TOF/MS and also the summary and discussion of the applications of the integrated strategy for HM qualitative analysis （2006-2011）. The advantages and future developments of LC coupled with IT and TOF-MS are highlighted.
基金supported by the Natural Science Foundation of Zhejiang Province,China (Y2080137)
文摘Euphorbia lathyris （Caper spurge） is a toxic and potent Chinese materia medica （T/PCMM）. This study sought a method for identifying five diterpenoids （Euphorbia factors LI-L3, L7a, and Ls） with the spectra of UV and mass, quantifying three diterpenoids L1, L2, and L8 in crude extracts of unprocessed and processed E. lathyris seeds by liquid chromatography/ electrospray ionization mass spectrometry （LC-ESI-MS）. The analysis was achieved on an Agilent Eclipse XDB-C18 column （4.6 mm× 150mm i.d., 5 μm） with an isocratic elution with a mobile phase consisting of water and acetonitrile at a flow rate of 0.25 mL/min at column temperature of 30 ℃ and UV detection was set at 272 nm. An ESI source was used with a positive ionization mode. The calibration curve was linear in the ranges of 9.9-79 μg/mL for Euphorbia factor Lb 3.8-30.5μg/mL for Euphorbia factor L2, and 1.0-20.6 μg/mL for Euphorbia factor LB. The average recoveries （n=6） of three diterpenoids were 98.39%, 91.10% and 96.94%, respectively, with RSD of 2.5%, 2.4% and 2.1%, respectively. The contents of the three diterpenoids in processed E. lathyris seeds were 3.435, 1.367 and 0.286 mg/g, respectively, which decreased more sharply than those in unprocessed E. lathyris seeds which were 4.915, 1.944 and 0.425 mg/g, respectively. The method is simple, accurate, reliable and reproducible, and it can be applied to control the quality of unprocessed and processed E. lathyris seeds.
文摘目的:比较试验和参比制剂2.5%复方利多卡因乳膏透皮作用的一致性。方法:以大鼠和巴马香猪的皮肤作为透皮渗透的材料,选用立式改良Franz扩散池测定复方利多卡因乳膏的渗透吸收规律,以高效液相色谱法分别测定接收液中药物的吸收总量和猪皮中药物的滞留量随时间的变化关系。结果:复方利多卡因乳膏试验与参比制剂在鼠皮及巴马香猪皮这两种不同透皮材料中5 h利多卡因的单位面积累积渗透量分别为(0.380±0.019)和(0.351±0.017)mg·cm^(-2),(0.228±0.012)和(0.217±0.023)mg·cm^(-2);丙胺卡因的单位面积累积渗透量分别为(0.422±0.022)和(0.382±0.029)mg·cm^(-2),(0.263±0.015)和(0.238±0.008)mg·cm^(-2);试验制剂与参比制剂在巴马香猪皮中5h的利多卡因,丙胺卡因的皮内滞留量分别为(2.021±0.094)和(1.999±0.118)mg·cm^(-2),(2.240±0.115)和(2.208±0.053)mg·cm^(-2);试验和参比制剂的体外释放比较的结果均符合FDA(U.S.Food and Drug Administration)和欧盟的指导原则。结论:2.5%复方利多卡因乳膏试验与参比制剂的透皮渗透程度和速率均符合外用制剂的一致性要求,且在猪皮内药物滞留特征相似。
