中国药房2017，Vol.28Issue(6)：803-808,6.DOI:10.6039/j.issn.1001-0408.2017.06.23
黄芩素中有关物质的检测及其降解机制初步研究
Detection of Related Substances and Preliminary Study on the Degradation Mechanism of Baicalein
摘要
Abstract
OBJECTIVE:To establish a method for the separation and detection of related substances in baicalein,identify its structure and preliminarily explore the degradation mechanism. METHODS:HPLC was adopted to detect the baicalein,related impurities and forced destruction of degradation products in synthesis process:the column was ES Industries? FluoroSep-RP Phenyl with mobile phase of 0.3%formic acid-methanol-acetonitrile(gradient elution)at a flow rate of 1.0 mL/min,the detection wavelength was 275 nm,the column temperature was 10℃,and the injection volume was 10μL. LC-MS/MS was conducted to identify the related substances and conjecture degradation mechanism:the column was ES Industries? FluoroSep-RP Phenyl with mobile phase of 0.3%formic acid- methanol (gradient elution)at a flow rate of 1.0 mL/min,the detection wavelength was 275 nm,column temperature was 10℃,and the injection volume was 10μL;ion source was electrospray ion source,positive and negative ions,nebulizer pressure was 55 psi and the drying gas flow was 11 L/min,drying gas temperature was 350℃,capillary voltage was 4.0 kV,detection modes were full-scan first-order MS and selective ion full-scan second-order MS,scan ranges were m/z 100-1000 (first-order MS) and 50-500(second-order MS),ionization voltage was 80-135 eV,and the collision energy was 10-30 eV. RESULTS:The linear range of baicalein was 2.4-480μg/mL(r=0.9999);RSDs of precision,stability and reproducibility tests were lower than 2.0%;the limit of quantitation was 7.2 ng,the limit of detection was 2.4 ng. Baicalein was well separated with related substance and 3 major degradation products,the related substance was chemical synthesis precursor wood butterfly;the degradation products were 6,7-quinone derivatives and 7,8-quinone derivatives,which were isomers;oxidative degradation products were benzoic acid phenyl ester derivatives. CONCLUSIONS:The main mechanisms of alkali degradation and oxidative degradation of baicalein include pyran, reciprocal rearrangement and oxidation reaction;the established method is specific and sensitive,and can be used for the detection of related substances in baicalein.关键词
黄芩素/有关物质/降解机制/高效液相色谱法/液相色谱-串联质谱法Key words
Baicalein/Related substance/Degradation mechanism/HPLC/LC-MS/MS分类
医药卫生引用本文复制引用
王玮珏,董武军,张培成,苏倩倩,范茹涵,刘玉玲..黄芩素中有关物质的检测及其降解机制初步研究[J].中国药房,2017,28(6):803-808,6.基金项目
"重大新药创制"科技重大专项(No.2012ZX09301002-001-008) （No.2012ZX09301002-001-008）
中央高校基本科研业务费专项"创新药物发现与新技术专项"(No.2012CHX03) （No.2012CHX03）
