Analytical Chemistry Department, Faculty of Pharmacy, Helwan University, Ein Helwan, 11795 Cairo, Egypt.
Analytical Chemistry Department, Faculty of Pharmacy, Helwan University, Ein Helwan, 11795 Cairo, Egypt; Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, October University for Modern Sciences and Arts (MSA), 11787 6 October City, Egypt.
J Chromatogr B Analyt Technol Biomed Life Sci. 2021 Aug 1;1179:122816. doi: 10.1016/j.jchromb.2021.122816. Epub 2021 Jul 6.
A simple, sensitive, rapid and specific method based on ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for the simultaneous quantification of dantrolene (DAN) and paracetamol (PAR) in real human plasma was developed and validated. The preparation of sample was achieved by liquid-liquid extraction with tertiary butyl methyl ether. The analysis was performed on a reversed-phase Ccolumn (1.7 µm, 2.1 × 30 mm) using acetonitrile: 0.1% formic acid (80:20, v/v) as the mobile phase and pumped in an isocratic mode at a flow rate of 0.3 mL/min using citalopram (CIT) as an internal standard. Tandem mass spectrometric detection was carried out by both positive and negative electrospray ionization (ESI) in the multiple-reaction monitoring mode (MRM). The analysis was carried out within 1 min for each sample which made it possible to analyze more than 350 human samples per day. Validation of the method was performed according to FDA guidelines for bio-analytical method. The method was found to be linear in the range of 25-2500 ng/mL and 100-10,000 ng/mL for DAN and PAR, respectively. The method was applied successfully for the determination of the two analytes in the plasma after oral administration of Dantrelax® compound capsules to healthy volunteers. The study was accomplished after approval of the ethics committee.
建立并验证了一种基于超高效液相色谱-串联质谱（UPLC-MS/MS）的简单、灵敏、快速和专属性强的方法，用于同时定量检测人血浆中的丹曲林（DAN）和对乙酰氨基酚（PAR）。样品制备采用叔丁基甲基醚进行液液萃取。采用反相 C 柱（1.7 µm，2.1×30 mm），以乙腈：0.1%甲酸（80:20，v/v）为流动相，以西酞普兰（CIT）为内标，以等度洗脱模式，流速为 0.3 mL/min 进行分析。采用正、负离子电喷雾电离（ESI）在多重反应监测模式（MRM）下进行串联质谱检测。每个样品的分析时间不到 1 分钟，每天可分析 350 多个人体样本。方法验证符合 FDA 对生物分析方法的指导原则。该方法在 25-2500 ng/mL 和 100-10,000 ng/mL 范围内，DAN 和 PAR 的线性良好。该方法成功应用于口服丹曲林复方胶囊后健康志愿者血浆中两种分析物的测定。该研究经伦理委员会批准后完成。
