高效液相色谱-串联质谱测定中草药中的赤霉素GA1、GA3、GA4、GA7  

Determination of GA1, GA3, GA4 and GA7 in Chinese Herbal Medicine byUltra Performance Liquid Chromatography Tandem Mass Spectrometry

作　　者：乔俊娟 余奕东[1] QIAO Jun-juan;YU Yi-dong(SGS-CSTC Standards Technical Services Co.,Ltd.,Guangzhou branch,Guangdong Guangzhou 510663,China)

机构地区：[1]通标标准技术服务有限公司广州分公司,广东广州510663

出　　处：《广州化工》2024年第6期154-157,186,共5页GuangZhou Chemical Industry

摘　　要：利用高效液相色谱-串联质谱技术建立测定中草药中赤霉素GA1、GA3、GA4、GA7残留的方法。样品经1%甲酸乙腈超声提取,氮吹浓缩后,以0.1%甲酸水-甲醇体系为流动相进行梯度洗脱,采用负离子质谱扫描模式进行监测,用基质匹配标准曲线定量。结果表明,4种赤霉素在5~100μg/L范围其线性相关系数大于0.995,检出限为0.005~0.01 mg/kg,定量限为0.025 mg/kg,在低、中、高3个水平的加标回收率在81.5%~115.8%之间,相对标准偏差小于8%,符合方法学验证要求。该方法前处理简单快速,准确性好,可用于筛查和检测中草药中赤霉素的残留。An Ultra-performance Liquid Chromatography-tandem Mass Spectrometry(UPLC-MS/MS)method was developed for the simultaneous determination of gibberellin A1(GA1),gibberellin A3(GA3),gibberellin A4(GA4)and gibberellin A7(GA7)in Chinese herbal medicine.Samples were ultrasohically extracted with acetonitrile containing 1%formic acid,concentrated by nitrogen purging.Gradient elution was performed with 0.1%formic acid aqueous solution containing methanol as the mobile phase.Mass spectrometry was conducted by electrospray ionization(ESI-)and multi response monitoring mode(MRM).The analyte was quantified by matrix-matching calibration curve.The final results were fairly linear in the range of 5~100μg/L,With correlation coefficients≥0.995.The detection limit was 0.005~0.01 mg/kg and the limit of quantification was 0.025 mg/kg.The average recoveries of all the samples were ranged from 81.5%~115.8%with the relative standard deviations(RSDs)≤8%at three spiked levels.The established method is simple quick and accurate,which can be applied to the analysis of the gibberellin residues in Chinese herbal medicine.

关 键 词：中草药 赤霉素 高效液相色谱-串联质谱(HPLC-MS/MS) 

分 类 号：O658[理学—分析化学]