8-O-乙酰山栀苷甲酯和山栀苷甲酯在大鼠体内的药代动力学分析
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摘要
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 develop UPLC-MS /MS for determination of 8-O-acetyl shanzhiside methyl ester and shanzhiside methyl ester in rat plasma and their pharmacokinetics study. Method: Plasma was precipitated with acetonitrile, mobile phase was consisted of acetonitrile and 0. 1% formic acid solution with gradient elution pumped at a flow rate of 0. 4 m L ·min- 1. Analysis was detected with positive electrospray ionization in multiple reaction monitoring( MRM) mode and rutin was used as internal standard. Result: Excellent linear calibration curves of 8-O-acetyl shanzhiside methyl ester and shanzhiside methyl ester were obtained in the concentration range of 1-250 μg·L- 1,their lower limits of quantification were 0. 2 μg·L- 1. Intra-day and interday relative standard deviations of low, medium and high quality control samples were all less than 8. 8%;Average recovery of 8-O-acetyl shanzhiside methyl ester were( 103. 89 ± 9. 18) %,( 99. 34 ± 6. 63) % and( 95. 88 ± 3. 69) %,while average recovery of shanzhiside methyl ester were( 105. 33 ± 8. 64) %,( 101. 55 ±1. 22) % and( 96. 89 ± 5. 42) %,respectively. Conclusion: This method is simple,rapid and sensitive,which is suitable for pharmacokinetics analysis of 8-O-acetyl shanzhiside methyl ester and shanzhiside methyl ester in rat plasma.
Objective: To develop UPLC-MS /MS for determination of 8-O-acetyl shanzhiside methyl ester and shanzhiside methyl ester in rat plasma and their pharmacokinetics study. Method: Plasma was precipitated with acetonitrile, mobile phase was consisted of acetonitrile and 0. 1% formic acid solution with gradient elution pumped at a flow rate of 0. 4 m L ·min- 1. Analysis was detected with positive electrospray ionization in multiple reaction monitoring( MRM) mode and rutin was used as internal standard. Result: Excellent linear calibration curves of 8-O-acetyl shanzhiside methyl ester and shanzhiside methyl ester were obtained in the concentration range of 1-250 μg·L- 1,their lower limits of quantification were 0. 2 μg·L- 1. Intra-day and interday relative standard deviations of low, medium and high quality control samples were all less than 8. 8%;Average recovery of 8-O-acetyl shanzhiside methyl ester were( 103. 89 ± 9. 18) %,( 99. 34 ± 6. 63) % and( 95. 88 ± 3. 69) %,while average recovery of shanzhiside methyl ester were( 105. 33 ± 8. 64) %,( 101. 55 ±1. 22) % and( 96. 89 ± 5. 42) %,respectively. Conclusion: This method is simple,rapid and sensitive,which is suitable for pharmacokinetics analysis of 8-O-acetyl shanzhiside methyl ester and shanzhiside methyl ester in rat plasma.
引文
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[9]王争,邓瑞雪,杨友亮,等.HPLC法同时测定糙苏中3个苯乙醇苷类化合物含量[J].药物分析杂志,2011,31(4):668-670.
[10]樊鹏程,李茂星,贾正平,等.RP-HPLC同时测定不同产地独一味药材中4种环烯醚萜苷[J].中草药,2010,41(3):483-485.
[11]尉丽力,邱建国,李茂星,等.独一味环烯醚萜苷胶囊质量标准研究[J].中国实验方剂学杂志,2013,19(22):137-140.
[12]袁涛,王森,管咏梅,等.HPLC同时测定奇正消痛贴膏中3种成分的含量[J].中国实验方剂学杂志,2014,20(19):72-75.
[13]郭伟一,卢胜明,廖立东,等.山栀苷甲酯在大鼠体内的药动学[J].中国新药与临床杂志,2013,32(12):993-997.
[2]袁涛,王森,顿珠,等.藏药独一味的研究进展[J].中成药,2014,36(9):1958-1961.
[3]潘正,高运玲,张涛,等.HPLC法测定独一味根中环烯醚萜苷和苯乙醇苷[J].中草药,2011,42(2):279-281.
[4]樊鹏程,马慧萍,景临林,等.反相制备液相色谱同时分离制备独一味中4种环烯醚萜苷类化合物[J].中草药,2012,43(4):699-701.
[5]高运玲,潘正,张涛,等.HPLC测定独一味不同制剂中4种环烯醚萜苷的含量[J].中成药,2010,32(1):71-74.
[6]邱建国,张泉龙,尉丽力,等.工业化提取分离纯化独一味总环烯醚萜苷类成分[J].中国实验方剂学杂志,2011,17(13):32-35.
[7]钟世红,古锐,王铃鑫,等.HPLC同时测定独一味中7种成分含量[J].中国中药杂志.2014,39(22):4373-4378.
[8]颜芳,曾光尧,谭健兵,等.植物中苯乙醇苷类化合物研究进展[J].中南药学,2013,11(5):358-362.
[9]王争,邓瑞雪,杨友亮,等.HPLC法同时测定糙苏中3个苯乙醇苷类化合物含量[J].药物分析杂志,2011,31(4):668-670.
[10]樊鹏程,李茂星,贾正平,等.RP-HPLC同时测定不同产地独一味药材中4种环烯醚萜苷[J].中草药,2010,41(3):483-485.
[11]尉丽力,邱建国,李茂星,等.独一味环烯醚萜苷胶囊质量标准研究[J].中国实验方剂学杂志,2013,19(22):137-140.
[12]袁涛,王森,管咏梅,等.HPLC同时测定奇正消痛贴膏中3种成分的含量[J].中国实验方剂学杂志,2014,20(19):72-75.
[13]郭伟一,卢胜明,廖立东,等.山栀苷甲酯在大鼠体内的药动学[J].中国新药与临床杂志,2013,32(12):993-997.