中国中药杂志

2018, v.43(06) 1156-1161

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UPLC-ELSD指纹图谱结合化学计量学方法用于骨刺片的质量控制
Quality control of Guci tablets using UPLC-ELSD fingerprint analysis coupled with chemometrics

王亚丹;戴忠;孙彩林;吴先富;马双成;
WANG Ya-dan;DAI Zhong;SUN Cai-lin;WU Xian-fu;MA Shuang-cheng;National Institutes for Food and Drug Control;

摘要(Abstract):

建立了骨刺片UPLC-ELSD指纹图谱分析方法,色谱柱为Waters Acquity UPLC BEH C_(18)柱(2.1 mm×100 mm,1.7μm),以0.1%甲酸水溶液-乙腈为流动相梯度洗脱,柱温30℃,流速0.3 m L·min~(-1),进样体积3μL,ELSD气体压力0.28 MPa,漂移管温度60℃,增益400。采用该方法测定6个厂家生产的39批骨刺片,并采用Chem Pattern软件进行分析。以75%以上样品中存在的色谱峰作为共有峰筛选条件,确定了30个共有峰,采用RRLC-MS/MS联用技术对其中19个共有峰进行指认,并对其中16个成分采用对照品比对的方式进行确证。样品与共有模式的相似度为0.47~0.98,表明不同厂家生产的骨刺片的质量相差较大,此外,对色谱数据进行主成分分析和聚类分析,阐明不同厂家制剂的主要差异性成分,结合这些成分的药材来源,推测部分厂家在三七、白芍和威灵仙投料方面可能存在问题,从而为骨刺片总体质量控制和标准提高提供参考。
Ultra-performance liquid chromatography-evaporative light scattering detection( UPLC-ELSD) fingerprint analysis method was established for quality control of Guci tablets. Chromatographic separation was performed on Waters Acquity UPLC BEH C_(18) column( 2. 1 mm × 100 mm,1. 7 μm) at 30 ℃ of column temperature. Acetonitrile-0. 1% formic acid solution was adopted as mobile phase for gradient elution. The flow rate was set at 0. 3 m L·min~(-1),and the injection volume was 3 μL. Detection was carried out on an ELSD with a nitrogen pressure of 0. 28 MPa,drift tube temperature of 60 ℃,and gain of 400. A total of 39 batches of samples produced by six manufacturers were measured by using the above method and the data were analyzed by Chem Pattern software. The peak present in more than 75% of the samples was defined as a common peak,and 30 common peaks were determined. Among them,19 peaks were identified by rapid resolution liquid chromatography/tandem mass spectrometry( RRLC-MS/MS) method,16 of which were confirmed by reference substances. The similarity of the tested samples was 0. 47-0. 98,suggesting that the quality of the samples from different manufacturers varied greatly. Furthermore,principal component analysis( PCA) and hierarchical analysis( HCA) were performed to clarify the main different components in samples. The results indicated that there might be some feeding problems about Paeoniae Radix Alba,Notoginseng Radix et Rhizoma,and Clematidis Radix et Rhizoma in a few manufacturers. This study provided some evidences for the overall quality control of Guci tablets,as well as its quality standard improvements.

关键词(KeyWords): 骨刺片;UPLC-ELSD;指纹图谱;化学计量学;质量控制
Guci tablets;UPLC-ELSD;fingerprint analysis;chemometrics;quality control

Abstract:

Keywords:

基金项目(Foundation):

作者(Author): 王亚丹;戴忠;孙彩林;吴先富;马双成;
WANG Ya-dan;DAI Zhong;SUN Cai-lin;WU Xian-fu;MA Shuang-cheng;National Institutes for Food and Drug Control;

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DOI: 10.19540/j.cnki.cjcmm.2018.0040

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