LC-MS/MS同时测定血浆中沙利度胺、来那度胺和波马多胺的含量

IF 1.3 4区 医学 Q4 PHARMACOLOGY & PHARMACY
Bin Wang , Wanting Qiang , Jia Yi , Shouhong Gao , Bosu Meng , Yuhui Mu , Bolong Wang , Zhipeng Wang , Xia Tao
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引用次数: 1

摘要

目的建立沙利度胺、来那度胺和波马多胺三种免疫调节剂的液相色谱-串联质谱(LC-MS/MS)定量分析方法。方法以沙利度胺-d4为内标,在Agilent Zorbax SB-C18(2.1 mm × 100 mm, 3.5 μm, Agilent, USA)色谱柱上分离,在Agilent G6460A三联四极杆质谱仪上多反应监测模式下进行监测。用3倍体积的甲醇对样品进行蛋白质沉淀预处理。流动相由0.1%甲酸水溶液(A相)和乙腈(B相)组成,以梯度洗脱程序输送。流速0.3 mL/min,进样量5 μL。结果该方法的准确度和稳定性在±15.0%以内,精密度不在15.0%以内。加样回收率为85.04% ~ 119.07%,基质效应为73.68% ~ 116.75%。特异性、线性度、定量限、结转、稀释度均符合药典和指南要求。沙利度胺、来那度胺的峰值浓度表现出巨大的个体间差异。结论该方法灵敏、简便、可靠,可用于多发性骨髓瘤患者三种免疫调节剂的治疗药物监测。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
Simultaneous quantification of thalidomide, lenalidomide and pomadomide in plasma by LC-MS/MS

Objective

To develop a new method for quantitatively analyzing three immunomodulators (thalidomide, lenalidomide and pomadomide) by liquid chromatography tandem mass spectrometry (LC-MS/MS).

Methods

Using thalidomide-d4 as internal standard, the three analytes were separated on Agilent Zorbax SB-C18(2.1 mm × 100 mm, 3.5 μm, Agilent, USA) column and monitored in multiple reactions monitoring mode in Agilent G6460A triple quadrupole mass spectrometer operating in positive ionization mode. The sample was pretreated by protein precipitation using methanol at 3-fold volume to sample. The mobile phase was comprised of 0.1% formic acid in water (phase A) and acetonitrile (phase B) and was delivered in gradient elution program. The flow rate was 0.3 mL/min, and the injection volume was 5 μL.

Results

The accuracy and stability of the method are within ±15.0%, and the precision is not >15.0%. The recoveries were 85.04% ∼ 119.07%, and the matrix effect was 73.68% ∼ 116.75%. Specificity, linearity, LLOQ, carry-over and dilution were all in line with the requirements of pharmacopeia and guidelines. The peak concentrations of thalidomide, lenalidomide shows huge inter-individual differences.

Conclusions

This newly developed method was sensitive, simple, and robust and can be used in therapeutic drug monitoring of three immunomodulators in multiple myeloma patients.

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来源期刊
Journal of pharmacological and toxicological methods
Journal of pharmacological and toxicological methods PHARMACOLOGY & PHARMACY-TOXICOLOGY
CiteScore
3.60
自引率
10.50%
发文量
56
审稿时长
26 days
期刊介绍: Journal of Pharmacological and Toxicological Methods publishes original articles on current methods of investigation used in pharmacology and toxicology. Pharmacology and toxicology are defined in the broadest sense, referring to actions of drugs and chemicals on all living systems. With its international editorial board and noted contributors, Journal of Pharmacological and Toxicological Methods is the leading journal devoted exclusively to experimental procedures used by pharmacologists and toxicologists.
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