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Simple, fast and robust LC-MS/MS method for the simultaneous quantification of canagliflozin, dapagliflozin and empagliflozin in human plasma and urine.
Journal of Chromatography B ( IF 2.8 ) Pub Date : 2020-06-26 , DOI: 10.1016/j.jchromb.2020.122257
Annemarie B van der Aart-van der Beek 1 , A Mireille A Wessels 2 , Hiddo J L Heerspink 2 , Daan J Touw 3
Affiliation  

Sodium–glucose cotransporter 2 –inhibitors (SGLT2i) are oral glucose-lowering drugs that have also demonstrated cardioprotective and renoprotective effects. SGLT2i play an increasingly important role in the treatment of type 2 diabetes. Here we report a simple and robust liquid chromatography–tandem mass spectrometry (LC–MS/MS) method for the simultaneous quantification of three SGLT2i (canagliflozin, dapagliflozin and empagliflozin) in human plasma, serum and urine with a runtime of 1 min. Methanol was used as protein precipitating agent. Chromatographic separation was accomplished using a Waters ACQUITY UPLC HSS T3 1.8 μm; 2.1 × 50 mm column with a Waters ACQUITY UPLC HSS T3 1.8 μm VanGuard Pre-column; 2.1 × 5 mm, using gradient elution with ammonium acetate 20 mM (pH 5) and acetonitrile as mobile phase at a flow rate of 0.8 ml/min. Mass spectrometric analysis of the acetate adduct ions was carried out using electrospray with negative ionization and SRM mode. The assay was validated according to FDA and EMA guidelines, including selectivity, linearity, accuracy and precision, dilution integrity, stability and recovery. With a sample volume of 200 µl, linear ranges of 10–5000 µg/L, 1–500 µg/L and 2–1000 µg/L for canagliflozin, dapagliflozin and empagliflozin respectively, were achieved. The assay was successfully applied in two pharmacokinetic studies with dapagliflozin and empagliflozin. In conclusion, we developed and validated a simple, fast and robust LC-MS/MS method for the simultaneous quantification of canagliflozin, dapagliflozin and empagliflozin, that allows rapid analysis of large numbers of samples and can be used for both pharmacokinetic studies and biomedical analysis of canagliflozin, dapagliflozin and empagliflozin.



中文翻译:

简单,快速,可靠的LC-MS / MS方法,可同时定量测定人血浆和尿液中的canagliflozin,dapagliflozin和empagliflozin。

钠葡萄糖共转运蛋白2抑制剂(SGLT2i)是口服降糖药物,也显示出心脏保护作用和肾脏保护作用。SGLT2i在2型糖尿病的治疗中起着越来越重要的作用。在这里,我们报告了一种简单而耐用的液相色谱-串联质谱(LC-MS / MS)方法,用于同时定量人血浆,血清和尿液中的三种SGLT2i(卡那列净,达格列净和恩格列净),时间为1分钟。甲醇用作蛋白质沉淀剂。使用Waters ACQUITY UPLC HSS T3 1.8μm色谱分离。2.1×50 mm色谱柱,带Waters ACQUITY UPLC HSS T3 1.8μmVanGuard预柱; 2.1×5毫米,使用20 mM醋酸铵(pH 5)和乙腈作为流动相的梯度洗脱,流速为0.8 ml / min。使用负离子化和SRM模式的电喷雾对乙酸加合物离子进行质谱分析。根据FDA和EMA指南对测定进行了验证,包括选择性,线性,准确性和精密度,稀释完整性,稳定性和回收率。对于200 µl的样品,canagliflozin,dapagliflozin和empagliflozin的线性范围分别为10–5000 µg / L,1–500 µg / L和2–1000 µg / L。该测定法已成功用于达格列净和依帕列净的两项药代动力学研究。总之,我们开发并验证了一种简单,快速且可靠的LC-MS / MS方法,用于同时定量测定canagliflozin,dapagliflozin和empagliflozin,

更新日期:2020-07-13
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