首页|LC-MS/MS法测定大鼠血浆中S,S,S-三丁基三硫代磷酸酯质量浓度及其毒物动力学研究

LC-MS/MS法测定大鼠血浆中S,S,S-三丁基三硫代磷酸酯质量浓度及其毒物动力学研究

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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 C18(50 mm×2。1 mm,3。5 μm)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2~800 μg·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。
Determination of S,S,S-tributyltrithiophosphate in rat plasma by LC-MS/MS and toxicokinetics study
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-C18 column(50×2.1 mm,3.5 μm).Mobile phase was 0.1%formic acid Water)-acetonitrile/methanol(V∶V=1∶1)withthegradient elution.Theflowratewasset at0.8 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 2-800 μg·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.

S,S,S-tirbutyltrithiophosphateLC-MS/MSplasmatoxicokinetic study

左琳、赵欣、杨巧惠、孙立新

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沈阳药科大学 药学院,辽宁 沈阳 110016

沈阳兴齐眼药股份有限公司,辽宁沈阳,110164

S,S,S-三丁基三硫代磷酸酯 LC-MS/MS 血浆 动力学研究

2024

沈阳药科大学学报
沈阳药科大学

沈阳药科大学学报

CSTPCD
影响因子:0.604
ISSN:1006-2858
年,卷(期):2024.41(6)