以研究白茶浸提液中杨梅素、槲皮素和山奈酚3种黄酮醇类物质的高效液相色谱(HPLC)检测方法及优化水解工艺为目的,通过精密度和加标回收率的测定,在确定HPLC检测方法可靠性的基础上,进一步采用正交试验法优化样品制备中的水解条件.结果表...以研究白茶浸提液中杨梅素、槲皮素和山奈酚3种黄酮醇类物质的高效液相色谱(HPLC)检测方法及优化水解工艺为目的,通过精密度和加标回收率的测定,在确定HPLC检测方法可靠性的基础上,进一步采用正交试验法优化样品制备中的水解条件.结果表明,制定的HPLC分离条件能有效分离芦丁、杨梅素、槲皮素和山奈酚,所得的标准曲线方程在线性范围内具有较高的精密度和加标回收率.白茶中3种黄酮醇类物质的最优水解工艺条件为:在5 m L白茶浸提液中添加5m L 3 mol·L-1盐酸,于80℃水浴锅中水解30 min.最优水解工艺的精密度均较高,在水解过程中山奈酚最稳定,杨梅素容易被分解,芦丁的水解转化率为94.32%.可见,将试验所得的HPLC检测方法及最优水解工艺用于测定白茶中黄酮醇类物质的含量是可行的,且可使白茶提取液中黄酮醇苷总量的水解趋于最大化.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
文摘以研究白茶浸提液中杨梅素、槲皮素和山奈酚3种黄酮醇类物质的高效液相色谱(HPLC)检测方法及优化水解工艺为目的,通过精密度和加标回收率的测定,在确定HPLC检测方法可靠性的基础上,进一步采用正交试验法优化样品制备中的水解条件.结果表明,制定的HPLC分离条件能有效分离芦丁、杨梅素、槲皮素和山奈酚,所得的标准曲线方程在线性范围内具有较高的精密度和加标回收率.白茶中3种黄酮醇类物质的最优水解工艺条件为:在5 m L白茶浸提液中添加5m L 3 mol·L-1盐酸,于80℃水浴锅中水解30 min.最优水解工艺的精密度均较高,在水解过程中山奈酚最稳定,杨梅素容易被分解,芦丁的水解转化率为94.32%.可见,将试验所得的HPLC检测方法及最优水解工艺用于测定白茶中黄酮醇类物质的含量是可行的,且可使白茶提取液中黄酮醇苷总量的水解趋于最大化.
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.
