柱前衍生化LC-MS/MS法测定大鼠血浆中丁香酚的质量浓度  

Determination of eugenol in rat plasma by LC-MS/MS with pre-column derivatization

作　　者：程聪 王鑫[1] 刘有平[1] 邸欣[1] CHENG Cong;WANG Xin;LIU Youping;DI Xin(School of Pharmacy,Shenyang Pharmaceutical University,Benxi 117004,China)

机构地区：[1]沈阳药科大学药学院,辽宁本溪117004

出　　处：《沈阳药科大学学报》2021年第3期251-257,共7页Journal of Shenyang Pharmaceutical University

摘　　要：目的建立灵敏、专属的柱前衍生化LC-MS/MS方法测定大鼠血浆中丁香酚的质量浓度。方法以麝香草酚为内标,血浆样品经丙酮沉淀蛋白和丹磺酰氯衍生化处理后,采用Key BDS Hypersil C8色谱柱(50 mm×4.6 mm,3μm)分离,以乙腈-水-甲酸(体积比85∶15∶0.5)为流动相进行等度洗脱,洗脱物通过电喷雾离子源正离子化后,以选择反应监测(SRM)模式进行扫描检测,用于定量分析的离子反应分别为m/z 398→m/z 171(丁香酚的衍生化产物)和m/z 384→m/z 171(内标的衍生化产物)。结果丁香酚在5.00~200μg·L^(-1)范围内呈良好线性关系(r≥0.9946),批内和批间精密度RSD小于7.7%,准确度RE值在2.3%~4.5%之间,提取回收率均在80.0%以上。结论本方法灵敏度高、选择性好,适用于大鼠血浆中丁香酚质量浓度的准确测定和以丁香为主药的中药方剂的药动学研究。Objective To establish a sensitive and selective method for determination of eugenol in rat plasma by LC-MS/MS with pre-column derivatization.Methods Using thymol as internal standard,the plasma samples were treated by protein precipitation method and separated on Key BDS Hypersil C8 column(50 mm×4.6 mm,3μm)after derivatization with dansyl chloride.The mobile phase was acetonitrile-water-formic acid(V∶V∶V=15∶85∶0.5)with the isocratic elution.The target compounds were determined in electrospray positive ionization(ESI+)and selective reaction monitoring(SRM)mode.The detected ions were m/z 398→m/z 171 for dansyl chloride derivative of eugenol and m/z 384→m/z 171 for dansyl chloride derivative of internal standard.Results The method was linear over the concentration ranges of 5.00-200μg·L^(-1)(r≥0.9946)for eugenol.The intra-day and inter-day precisions were less than 7.7%,the accuracy was between 2.3%and 4.5%,and the extraction recovery was above 80%.Conclusion The method had the advantages of high sensitivity and good selectivity.It was suitable for the accurate determination of eugenol in rat plasma and the pharmacokinetics analysis of traditional Chinese medicine prescription with clove as the monarch.

关 键 词：丁香酚 衍生化 液相色谱-串联质谱法 血浆 

分 类 号：R917[医药卫生—药物分析学]