Determination of Tacrolimus in Plasma by Supramolecular Solvent Extraction/Ultra-high Performance Liquid Chromatography－ Tandem Mass Spectrometry

XIE Yi-qing; LÜ Yue-guang; MENG Xian-shuang; LEI Hai-min; MA Qiang

doi:10.19969/j.fxcsxb.23011103

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Determination of Tacrolimus in Plasma by Supramolecular Solvent Extraction/Ultra-high Performance Liquid Chromatography－ Tandem Mass Spectrometry

Scientific Papers | 更新时间：2023-05-15

- Determination of Tacrolimus in Plasma by Supramolecular Solvent Extraction/Ultra-high Performance Liquid Chromatography－ Tandem Mass Spectrometry
- Journal of Instrumental Analysis Vol. 42, Issue 5, Pages: 559-567(2023)
- 作者机构：
  
  1.北京中医药大学中药学院，北京 102488
  2.中国检验检疫科学研究院，北京 100176
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.23011103
  CLC：
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谢以清,吕悦广,孟宪双等.超分子溶剂萃取/超高效液相色谱－串联质谱法测定血浆中他克莫司含量[J].分析测试学报,2023,42(05):559-567.

XIE Yi-qing,LÜ Yue-guang,MENG Xian-shuang,et al.Determination of Tacrolimus in Plasma by Supramolecular Solvent Extraction/Ultra-high Performance Liquid Chromatography－ Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2023,42(05):559-567.
谢以清,吕悦广,孟宪双等.超分子溶剂萃取/超高效液相色谱－串联质谱法测定血浆中他克莫司含量[J].分析测试学报,2023,42(05):559-567. DOI： 10.19969/j.fxcsxb.23011103.

XIE Yi-qing,LÜ Yue-guang,MENG Xian-shuang,et al.Determination of Tacrolimus in Plasma by Supramolecular Solvent Extraction/Ultra-high Performance Liquid Chromatography－ Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2023,42(05):559-567. DOI： 10.19969/j.fxcsxb.23011103.

摘要

该文建立了血浆中免疫抑制剂他克莫司（TAC）的超分子溶剂（SUPRAS）萃取/超高效液相色谱－串联质谱分析方法。通过单因素实验结合响应面设计对超分子溶剂组成、用量及涡旋萃取时间等关键因素进行优化后，血浆样本以正戊醇、四氢呋喃和水形成的超分子溶剂进行高效萃取。萃取液经Waters ACQUITY UPLC BEH C,18,（50 mm × 2.1 mm，1.7 μm）色谱柱分离后，在电喷雾质谱正离子模式下，以多反应监测（MRM）模式对他克莫司进行测定，内标法定量。结果表明，他克莫司在0.5 ~ 30 ng/mL质量浓度范围内的线性关系良好，相关系数（,r,）为0.998 6；方法检出限和定量下限分别为0.1、0.5 ng/mL；在低、中、高3个加标水平下，平均回收率（,n ,= 3）为91.9% ~ 99.9%，相对标准偏差（RSD）为1.7% ~ 5.7%。所建立的方法快速、灵敏、稳定，适用于血浆中他克莫司的准确测定。

Abstract

An analytical method for the determination of tacrolimus（TAC） in blood plasma was established by supramolecular solvent（SUPRAS） extraction combined with ultra-high performance liquid chromatography－tandem mass spectrometry．After optimizing the key factors such as the composition and amount of SUPRAS，and vortex extraction time through single factor experiment and response surface design，blood plasma samples were extracted efficiently with SUPRAS formed by pentanol，tetrahydrofuran and water．The extract was separated on a Waters ACQUITY UPLC BEH C,18, column（50 mm × 2.1 mm，1.7 μm），analyzed by electrospray ionization mass spectrometry in positive ion mode under multiple reaction monitoring（MRM） mode，and quantified by internal standard method．Experimental results demonstrated that there was a good linear relationship for TAC in the concentration range of 0.5－30 ng/mL，with a correlation coefficient（,r,） of 0.998 6．The limit of detection（LOD） and quantitation（LOQ） were 0.1 ng/mL and 0.5 ng/mL，respectively．The average recoveries（,n ,= 3） at low，medium and high spiked concentration levels ranged from 91.9% to 99.9%，with relative standard deviations（RSDs） of 1.7%－5.7%．The proposed method is rapid，sensitive and stable，and it was suitable for the accurate determination of TAC in blood plasma.

关键词

他克莫司免疫抑制剂超分子溶剂血浆超高效液相色谱－串联质谱

Keywords

tacrolimusimmunosuppresive agentsupramolecular solventplasmaultra-high performance liquid chromatography－tandem mass spectrometry

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