Maráková K, Piestanský J, Havránek E, Mikus P
Pharmazie. 2014 Sep;69(9):663-8.
The advanced hyphenated method based on capillary electrophoresis (CE) on-line combined with electrospray ionization (ESI) and tandem mass spectrometry (MS/MS, here triple quadrupole, QqQ) was developed and applied in pharmaceutical analysis in this work. Under the optimized CE separation (background electrolyte: 50 mmol/L formic acid with pH 2.05), ESI ionization (sheath liquid: 0.1% v/v formic acid in 50% v/v aq methanol) and QqQ detection (100-160V fragmentor voltage, 15-25eV collision energy, depending on the type of analyte) conditions, highly efficient, reproducible, accurate, sensitive (sub microg/mL LODs) and selective (each analyte was unequivocally specified by two characteristic MS signals, i.e. qualifier, quantifier) determination of vitamins B was achieved. All vitamins B, namely thiamine, riboflavin, nicotinamide, nicotinic acid, pantothenic acid, pyridoxine, biotin, folic acid and cyanocobalamine, were simultaneously determined in various dosage forms (injection solution, tablets, and effervescent tablets) within ca. 16 min. The main benefits of the proposed CE-ESI-QqQ method in comparison with the CE-UV ones are considerably enhanced sensitivity and selectivity. Other benefits are low cost, simplicity, flexibility and environmental aspects when comparing CE-ESI-QqQ with HPLC-MS. Successful validation and application of the proposed CE-ESI-QqQ method suggest its routine use in highly effective and reliable multi-drug quality control.
本文开发了一种基于毛细管电泳(CE)在线联用电喷雾电离(ESI)和串联质谱(MS/MS,此处为三重四极杆,QqQ)的先进联用方法,并将其应用于药物分析。在优化的CE分离条件(背景电解质:50 mmol/L甲酸,pH 2.05)、ESI电离条件(鞘液:50% v/v甲醇水溶液中含0.1% v/v甲酸)和QqQ检测条件(100 - 160V碎裂电压,15 - 25eV碰撞能量,取决于分析物类型)下,实现了对维生素B的高效、可重现、准确、灵敏(检测限低至亚微克/毫升)和选择性(每种分析物由两个特征性MS信号明确指定,即定性离子、定量离子)测定。所有维生素B,即硫胺素、核黄素、烟酰胺、烟酸、泛酸、吡哆醇、生物素、叶酸和氰钴胺素,均可在约16分钟内同时测定各种剂型(注射液、片剂和泡腾片)中的含量。与CE - UV方法相比,所提出的CE - ESI - QqQ方法的主要优点是灵敏度和选择性大大提高。与HPLC - MS相比,其他优点包括成本低、操作简单、灵活性高以及环保。所提出的CE - ESI - QqQ方法的成功验证和应用表明其可常规用于高效可靠的多药物质量控制。