A rapid, reliable, and sensitive method was developed using ultra-performance liquid chromatography- tandem mass spectrometry （UPLC-MS/MS） with an electrospray ionization （ESI） source for determination of seven bi...A rapid, reliable, and sensitive method was developed using ultra-performance liquid chromatography- tandem mass spectrometry （UPLC-MS/MS） with an electrospray ionization （ESI） source for determination of seven bioactive compounds in rat plasma after oral administration of Ginkgo biloba tablets （GBTs）. The method simultane- ously detects bilobalide （BB）, ginkgolide A （GA）, ginkgolide B （GB）, ginkgolide C （GC）, quercetin （QCT）, kaempferol （KMF）, and isorhamnetin （ISR） for pharmacokinetic study. The analytes and internal standard （IS） were extracted from rat plasma by acetidin. An MS/MS detection was conducted using multiple reaction monitoring （MRM） and operating in the negative ionization mode. The calibration curve ranges were 5-500, 5-500, 2.5-250, 1-100, 1-100, 1-100, and 1-100 ng/ml for BB, GA, GB, GC, QCT, KMF, and ISR, respectively. The mean recovery of the analytes ranged from 68.11% to 84.42%. The intra- and inter-day precisions were in the range of 2.33%-9.86% and the accuracies were between 87.67% and 108.37%. The method was used successfully in a pharmacokinetic study of GBTs. The phar- macokinetic parameters of seven compounds were analyzed using a non-compartment model. Plasma concentrations of the seven compounds were determined up to 48 h after administration, and their pharmacokinetic parameters were in agreement with previous studies.展开更多
Total flavonoid glycoside was isolated from Ginkgo biloba Linn. leaf tablet and determined by RP-HPLC using quercetin as external standard. 4.6 mm×100 mm Spherisorb ODS column, mobile phase: V (CH\-\{3\}OH) ∶ V ...Total flavonoid glycoside was isolated from Ginkgo biloba Linn. leaf tablet and determined by RP-HPLC using quercetin as external standard. 4.6 mm×100 mm Spherisorb ODS column, mobile phase: V (CH\-\{3\}OH) ∶ V (0.3% H\-\{3\}PO\-\{4\})=40∶60, flow rate: 1 mL/min, detection: λ=370 nm. The sample was extracted with CH\-\{3\}OH by ultrasonic extraction and hydrolyzed with 25% HCl, then sample solution was diluted accurately to 50 mL. This experiment showed that this is a simple, accurate and precise method with the result of fine linearity, average recovery is 101.1% for quercetin, and RSD is 2.44%.展开更多
基金supported by the National Basic Research Program(973) of China(No.2012CB724001)the National Natural Science Foundation of China(No.81473365)+2 种基金the Beijing Natural Science Foundation of China(No.7132172)the Independent Project of Beijing University of Chinese Medicine(No.2014-JYBZZ-XS-106)the Innovative Research Team of Beijing University of Chinese Medicine(No.2011-CXTD-13),China
文摘A rapid, reliable, and sensitive method was developed using ultra-performance liquid chromatography- tandem mass spectrometry （UPLC-MS/MS） with an electrospray ionization （ESI） source for determination of seven bioactive compounds in rat plasma after oral administration of Ginkgo biloba tablets （GBTs）. The method simultane- ously detects bilobalide （BB）, ginkgolide A （GA）, ginkgolide B （GB）, ginkgolide C （GC）, quercetin （QCT）, kaempferol （KMF）, and isorhamnetin （ISR） for pharmacokinetic study. The analytes and internal standard （IS） were extracted from rat plasma by acetidin. An MS/MS detection was conducted using multiple reaction monitoring （MRM） and operating in the negative ionization mode. The calibration curve ranges were 5-500, 5-500, 2.5-250, 1-100, 1-100, 1-100, and 1-100 ng/ml for BB, GA, GB, GC, QCT, KMF, and ISR, respectively. The mean recovery of the analytes ranged from 68.11% to 84.42%. The intra- and inter-day precisions were in the range of 2.33%-9.86% and the accuracies were between 87.67% and 108.37%. The method was used successfully in a pharmacokinetic study of GBTs. The phar- macokinetic parameters of seven compounds were analyzed using a non-compartment model. Plasma concentrations of the seven compounds were determined up to 48 h after administration, and their pharmacokinetic parameters were in agreement with previous studies.
文摘Total flavonoid glycoside was isolated from Ginkgo biloba Linn. leaf tablet and determined by RP-HPLC using quercetin as external standard. 4.6 mm×100 mm Spherisorb ODS column, mobile phase: V (CH\-\{3\}OH) ∶ V (0.3% H\-\{3\}PO\-\{4\})=40∶60, flow rate: 1 mL/min, detection: λ=370 nm. The sample was extracted with CH\-\{3\}OH by ultrasonic extraction and hydrolyzed with 25% HCl, then sample solution was diluted accurately to 50 mL. This experiment showed that this is a simple, accurate and precise method with the result of fine linearity, average recovery is 101.1% for quercetin, and RSD is 2.44%.
