摘要
目的 建立LC-MS/MS法测定大鼠血浆中S,S,S-三丁基三硫代磷酸酯的质量浓度,并用于大鼠体内的毒物动力学研究。方法 采用沉淀蛋白法进行血浆样品前处理,以丙酸倍氯米松为内标。色谱柱为Agilent Zorbax SB C_(18)(50 mm×2.1 mm, 3.5μm)柱,流动相为水(含体积分数0.1%甲酸)-乙腈/甲醇(体积比1∶1),梯度洗脱,流速为0.8 mL·min^(-1)。质谱检测采用ESI源,正离子化方式,多反应监测模式(MRM)进行扫描检测。结果 血浆中S,S,S-三丁基三硫代磷酸酯线性范围为2~800μg·L^(-1),线性良好(r≥0.99),批内、批间RSD均在±15%内,准确度在85%~115%内。高、中、低质量浓度总体提取回收率为89.0%,变异系数为1.1%。结论 本方法适用于大鼠血浆中S,S,S-三丁基三硫代磷酸酯质量浓度的准确测定和动力学研究。
Objective To establish a specific and sensitive LC-MS/MS method for determination of S,S,S-tributyltrithiophosphate in rat plasma and its application for toxicokinetic study.Methods Plasma samples were pretreated by protein precipitation method using beclomethasone as internal standard.Sample separation was carried on Agilent Zorbax SB-C_(18)column(50×2.1 mm,3.5μm).Mobile phase was 0.1% formic acid Water)-acetonitrile/methanol(V∶V=1∶1)with the gradient elution.The flow rate was set at 0.8 mL·min^(-1).The positive ionization mode of electrospray(ESI)source was used by multiple reaction monitoring(MRM).Results The method was linear over the concentration ranges of 2-800μg·L^(-1)(r≥0.99).The accuracy(RE)and inter/intra day precision(RSD)was both within±15%.The overall recovery was 89.0%,and the CV was 1.1%.Conclusion The method was rapid,sensitive and reliable,and could be applied successfully for determination of S,S,S-tributyltrithiophosphate in rat plasma and toxicokinetic study.
作者
左琳
赵欣
杨巧惠
孙立新
ZUO Lin;ZHAO Xin;YANG Qiaohui;SUN Lixin(School of Pharmacy,Shenyang Pharmaceutical University,Shenyang 110016,China;Shenyang Sinqi Pharmaceutical,LtdcoShenyang 110164,China)
出处
《沈阳药科大学学报》
CAS
CSCD
2024年第6期720-725,共6页
Journal of Shenyang Pharmaceutical University
作者简介
左琳(1991-),女(汉族),辽宁沈阳人,本科,E-mail:1596401088@qqcom;通信作者:孙立新(1967-),女(汉族),辽宁新宾人,博士,教授,博士研究生导师,主要从事化学药和中药的药物分析学、代谢组学方向的研究,E-mail:slx04@163com。
