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目的:建立超高效液相串联质谱法(UPLC-MS/MS)同时检测大鼠体内8-O-乙酰山栀苷甲酯和山栀苷甲酯血药浓度的方法,并考察二者在大鼠体内的药代动力学过程。方法:利用乙腈沉淀蛋白法处理血浆样品,检测条件为流动相乙腈(A)-0.1%甲酸水溶液(B)梯度洗脱(0~1.5 min,20%~60%A;1.5~2 min,60%~95%A;2~2.5 min,95%A;2.5~2.6 min,95%~20%A;2.6~3 min,20%A),流速0.4 m L·min-1,柱温40℃,进样量2μL,内标物为芦丁;采用正离子多离子反应监测(MRM)扫描。结果:血浆中8-O-乙酰山栀苷甲酯和山栀苷甲酯的线性范围均为1~250μg·L-1,定量下限均为0.2μg·L-1。低、中、高质量浓度8-O-乙酰山栀苷甲酯和山栀苷甲酯质控样品的日内、日间精密度RSD均<8.8%;8-O-乙酰山栀苷甲酯的相对回收率依次为(103.89±9.18)%,(99.34±6.63)%和(95.88±3.69)%;山栀苷甲酯的相对回收率分别为(105.33±8.64)%,(101.55±1.22)%和(96.89±5.42)%。结论:该方法操作简便、快捷、灵敏度高,适用于大鼠血浆中8-O-乙酰山栀苷甲酯和山栀苷甲酯的药代动力学研究。
OBJECTIVE: To establish a method for the simultaneous determination of 8-O-acetylglucoside methyl and methylglucoside methyl ester concentrations in rat by UPLC-MS / MS. Pharmacokinetics in rats. Methods: The plasma samples were processed by acetonitrile precipitating protein. The mobile phase consisted of acetonitrile (A) - 0.1% formic acid (B) gradient elution (0 ~ 1.5 min, 20% ~ 60% A; % ~ 95% A; 2 ~ 2.5 min, 95% A; 2.5 ~ 2.6 min, 95% ~ 20% A; 2.6 ~ 3 min, 20% , Injection volume 2μL, internal standard rutin; positive ion multi-ion reaction monitoring (MRM) scan. Results: The linear ranges of 8-O-acetylglucoside methyl ester and gossypin methyl ester in plasma were both 1 ~ 250μg · L-1, and the lower limit of quantification was 0.2μg · L-1. The RSDs of intra-day and inter-day precision of low, middle and high quality concentration 8-O-acetylglucoside methyl ester and androsterone methyl ester control samples were all less than 8.8%. The 8-O-acetylglucoside methyl ester The relative recoveries were (103.89 ± 9.18)%, (99.34 ± 6.63)% and (95.88 ± 3.69)%, respectively. The relative recoveries of the two compounds were 105.33 ± 8.64% and 101.55 ± 1.22% And (96.89 ± 5.42)% respectively. Conclusion: The method is simple, rapid and sensitive. It is suitable for the pharmacokinetic study of 8-O-acetylglucoside methyl ester and gossypin methyl ester in rat plasma.