采用非水反相高效液相色谱法（NARP-HPLC）和大气压化学电离质谱法（APCI-MS）同时分离和测定辅酶Q(10)及其工艺相关杂质。

Simultaneous separation and determination of coenzyme Q(10) and its process related impurities by NARP-HPLC and atmospheric pressure chemical ionization-mass spectrometry (APCI-MS).

作者信息

Nageswara Rao R, Kumar Talluri M V Narendra, Shinde Dhananjay D

机构信息

Analytical Chemistry Division, Discovery Laboratory, Indian Institute of Chemical Technology, Tarnaka, Hyderabad, India.

出版信息

J Pharm Biomed Anal. 2008 Jun 9;47(2):230-7. doi: 10.1016/j.jpba.2007.12.034. Epub 2007 Dec 27.

DOI:10.1016/j.jpba.2007.12.034

PMID:18243624

Abstract

A non-aqueous reversed phase high performance liquid chromatographic (NARP-HPLC) method for determination of coenzyme Q(10) in pharmaceutical preparations has been developed using Kromosil C(8) column with acetonitrile and isopropyl alcohol (84:16, v/v) as a mobile phase. Photodiode array (PDA) detector set at 210 nm was used for monitoring of the eluents. The method is simple, rapid, selective and capable of separating all process impurities at trace level with detection limits <0.1 microg/ml. It has been validated with respect to accuracy, precision, linearity, and limits of detection and quantification. The linearity range was 50-300 microg/ml. The percentage recoveries ranged from 95.10 to 101.02. The method was found to be suitable not only for monitoring the reactions during the process development but also quality assurance of coenzyme Q(10). For identification of related substances atmospheric pressure chemical ionisation-mass spectrometry (APCI-MS) was used.

摘要

已开发出一种用于测定药物制剂中辅酶Q(10)的非水反相高效液相色谱法（NARP-HPLC），该方法使用Kromosil C(8)柱，以乙腈和异丙醇（84:16，v/v）作为流动相。采用设置在210 nm的光电二极管阵列（PDA）检测器监测洗脱液。该方法简单、快速、具有选择性，能够分离痕量水平的所有工艺杂质，检测限<0.1 μg/ml。已对该方法的准确性、精密度、线性以及检测限和定量限进行了验证。线性范围为50-300 μg/ml。回收率在95.1%至101.02%之间。该方法不仅适用于监测工艺开发过程中的反应，也适用于辅酶Q(10)的质量保证。使用大气压化学电离质谱法（APCI-MS）鉴定相关物质。