建立并验证了一种快速高效液相色谱-串联质谱法，可同时测定全血中环孢素 A 和他克莫司的浓度，用于器官移植患者的常规治疗药物监测。
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.
机构信息
Beijing Chao-Yang Hospital, Capital Medical University, Beijing, China.
出版信息
Rapid Commun Mass Spectrom. 2025 Jan 30;39(2):e9932. doi: 10.1002/rcm.9932.
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 ZnSO. Chromatography was performed on a pre-column using a gradient elution with 20 mmol. L 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. 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 for tacrolimus and 50 ng. L 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-, 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.
背景
治疗药物监测是器官移植的一个组成部分。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，用于同时测定免疫抑制剂环孢素 A 和他克莫司，可能会提高检测效率。
方法
本研究建立并验证了一种快速的 HPLC-MS/MS 方法。通过用乙腈和 0.5 mol.L ZnSO 沉淀蛋白，制备 100 μL 的全血样本。使用预柱，在 20 mmol.L 甲酸铵和 0.1%（v/v）甲酸的水溶液（流动相 A）和 0.1%（v/v）甲酸的甲醇溶液（流动相 B）中进行梯度洗脱，流速为 1.5 mL.min。分析时间为 2.2 min。采用电喷雾电离和多反应监测进行分析。他克莫司和环孢素 A 的定量下限分别设定为 1 ng.L 和 50 ng.L。
结果
该方法具有足够的线性范围和良好的准确性和精密度。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>0.99。
结论
所建立的 HPLC-MS/MS 方法快速，可用于同时监测他克莫司和环孢素 A。
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