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Simultaneous Determination of Six Immunosuppressants in Human Whole Blood by HPLC-MS/MS Using a Modified QuEChERS Method.
Zheng, Min; Song, Jianshi; Xue, Hua; Li, Hui; Lian, Kaoqi.
Afiliação
  • Zheng M; School of Public Health, Hebei Medical University, Shijiazhuang 050017, China.
  • Song J; Jinan Center for Disease Control and Prevention, Jinan 250000, China.
  • Xue H; The School of Basic Medicine, Hebei Medical University, Shijiazhuang 050017, China.
  • Li H; Chemistry Teaching Group and Fundamental Medical Department, Shijiazhuang 050599, China.
  • Lian K; Hebei Institute for Drug and Medical Device Control, Shijiazhuang 050299, China.
Molecules ; 27(13)2022 Jun 25.
Article em En | MEDLINE | ID: mdl-35807333
ABSTRACT
A high-performance liquid chromatography-tandem mass spectrometry method was established for the simultaneous determination of mycophenolic acid, mycophenolate mofetil, tacrolimus, rapamycin, everolimus and pimecrolimus in human whole blood by optimizing the QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) preparation method. Whole blood was extracted into ethyl acetate, salted out with anhydrous magnesium sulfate, and purified with ethylenediamine-N-propyl silane adsorbent. The supernatant was evaporated under nitrogen until dry and finally reconstituted in methanol. Chromatographic separation was performed on an Agilent Poroshell 120 EC-C18 column in methanol (mobile phase A)-water (optimized for 0.1% acetic acid and 10 mM ammonium acetate, mobile phase B) at a 0.3 mL·min−1 flow rate. Electrospray ionization and positive ion multiple reaction monitoring were used for detection. The time for of analysis was 13 min. The calibration curves range of tacrolimus, rapamycin, everolimus and pimecrolimus were in the range of 1−100 ng·mL−1, mycophenolate mofetil in the range of 0.1−10 ng·mL−1 and mycophenolic acid at 10−1000 ng·mL−1. All correlation coefficients were >0.993. The coefficients of variation (CV, %) for inter-day and intra-day precision were less than 10%, while the spiked recoveries were in the range of 92.1% to 116%. Our method was rapid, sensitive, specific, and reproducible for the simultaneous determination of six immunosuppressants in human whole blood. Importantly, our approach can be used to monitor drug concentrations in the blood to facilitate disease treatment.
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Texto completo: 1 Base de dados: MEDLINE Assunto principal: Espectrometria de Massas em Tandem / Imunossupressores Limite: Humans Idioma: En Ano de publicação: 2022 Tipo de documento: Article

Texto completo: 1 Base de dados: MEDLINE Assunto principal: Espectrometria de Massas em Tandem / Imunossupressores Limite: Humans Idioma: En Ano de publicação: 2022 Tipo de documento: Article