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Determination of ergocalciferol in human plasma after Diels-Alder derivatization by LC-MS/MS and its application to a bioequivalence study

查看全文 作　　者：Pritesh [1,2]Contractor;Abhishek [2]Gandhi;Gajendra [2]Solanki;Priyanka A. [3]Shah;Pranav S. [3]Shrivastav 高影响力作者 机构地区：[1]Department of Chemistry, Kadi Sarva Vishwavidyalaya, Gandhinagar, Ahmedabad-382015, India;[2]Bioanalytical Department, Veeda Clinical Research, Ahmedabad-387810, India;[3]Department of Chemistry, School of Sciences, Gujarat University, Ahmedabad-380009, India高影响力机构 出　　处：《Journal of Pharmaceutical Analysis》索引2017年第7卷第6期,共6页高影响力期刊 摘　　要：An accurate, sensitive and selective method is developed for determination of ergocalciferol(vitamin D_2) in human plasma using LC–MS/MS. After liquid-liquid extraction with n-hexane, ergocalciferol was derivatized by reacting with 4-phenyl-1,2,4-triazoline-3,5-dione(PTAD), a strong dienophile based on Diels-Alder reaction.Ergocalciferol and its deuterated internal standard, ergocalciferol-d6, were analyzed on X Select CSH C_(18)(100 mm×4.6 mm, 2.5 μm) column using acetonitrile and 0.1%(v/v) formic acid in water containing 0.14% methylamine within 6.0 min under gradient elution mode. Tandem mass spectrometry in positive ionization mode was used to quantify ergocalciferol by multiple reaction monitoring(MRM). Entire data processing was done using Watson LIMS^(TM) software which provided excellent data integrity and high throughput with improved operational efficiency. The major advantage of this method includes higher sensitivity(0.10 ng/mL),superior extraction efficiency(≥83%) and small sample volume(100 μL) for processing. The method was linear in the concentration range of 0.10–100 ng/mL for ergocalciferol. The intra-batch and inter-batch accuracy and precision(% CV) values varied from 97.3% to 109.0% and 1.01% to 5.16%, respectively. The method was successfully applied to support a bioequivalence study of 1.25 mg ergocalciferol capsules in 12 healthy subjects. 关 键 词：ERGOCALCIFEROL 一天一夜桤木的反应 4-phenyl-1,2,4-triazoline-3,5-dione LC-MS/MS 人的血浆
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