开发并验证一种快速 HPLC-MS/MS 方法,用于同时测定全血中的环孢素 A 和他克莫司,以监测器官移植中的常规治疗药物。

IF 1.8 3区 化学 Q4 BIOCHEMICAL RESEARCH METHODS
Fei-fei Han, Hong-chuan Liu, Ting Hu, Peng-fei Li, Rui Zhao, Zhuo-ling An
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引用次数: 0

摘要

背景:治疗药物监测是器官移植不可或缺的一部分。一种快速、简单、经济、稳健的高效液相色谱-串联质谱(HPLC-MS/MS)方法可同时测定免疫抑制剂环孢素 A 和他克莫司,从而提高检测效率:本研究开发并验证了一种快速 HPLC-MS/MS 方法。全血样品 100 μL 用乙腈和 0.5 mol.L-1 ZnSO4沉淀蛋白质。在预柱上用 20 mmol.L-1 甲酸铵和 0.1% (v/v) 甲酸水(流动相 A)以及 0.1% (v/v) 甲酸甲醇(流动相 B)进行梯度洗脱,流速为 1.5 mL.min-1。分析时间为 2.2 分钟。进行了电喷雾离子化和多反应监测。他克莫司的定量下限为 1 纳克/升-1。L-1,环孢素 A 为 50 ng。L-1:该方法准确度和精密度良好,线性范围足够宽。他克莫司和环孢素 A 的校准曲线范围分别为 1-30 和 50-1500 ng-mL-1。所有相关系数均大于 0.99:所开发的高效液相色谱-质谱/串联质谱法速度快,可用于他克莫司和环孢素 A 的同时监测。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
Development and validation of a rapid HPLC-MS/MS method for simultaneous determination of cyclosporine A and tacrolimus in whole blood for routine therapeutic drug monitoring in organ transplantation

Background

Therapeutic drug monitoring is an integral part of organ transplantation. A rapid, simple, economical, and robust high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for simultaneously determining the immunosuppressants cyclosporine A and tacrolimus might increase detection efficiency.

Methods

In this study, we developed and validated a rapid HPLC-MS/MS method. Whole blood samples of 100 μL were prepared by protein precipitation with acetonitrile and 0.5 mol. L−1 ZnSO4. Chromatography was performed on a pre-column using a gradient elution with 20 mmol. L−1 ammonium formate and 0.1% (v/v) formic acid in water (mobile phase A) and 0.1% (v/v) formic acid in methanol (mobile phase B) at a flow rate of 1.5 mL.min−1. The analysis time was 2.2 min. Electrospray ionization and multiple reaction monitoring were performed. The lower limit of quantification was set at 1 ng. L−1 for tacrolimus and 50 ng. L−1 for cyclosporine A.

Results

The method showed adequate accuracy and precision with a sufficient linear range. The calibration curve range of tacrolimus and cyclosporine A was 1–30 and 50–1500 ng·mL-1, respectively. All correlation coefficients were >0.99.

Conclusions

The developed HPLC-MS/MS is rapid and can be used for simultaneous monitoring of tacrolimus and cyclosporine A.

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来源期刊
CiteScore
4.10
自引率
5.00%
发文量
219
审稿时长
2.6 months
期刊介绍: Rapid Communications in Mass Spectrometry is a journal whose aim is the rapid publication of original research results and ideas on all aspects of the science of gas-phase ions; it covers all the associated scientific disciplines. There is no formal limit on paper length ("rapid" is not synonymous with "brief"), but papers should be of a length that is commensurate with the importance and complexity of the results being reported. Contributions may be theoretical or practical in nature; they may deal with methods, techniques and applications, or with the interpretation of results; they may cover any area in science that depends directly on measurements made upon gaseous ions or that is associated with such measurements.
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