摘要
利用免疫亲和萃取结合超高效液相色谱-串联四极杆质谱技术(UHPLC-E S I/Q qQ-M S/M S)建立了中成药及中药材中5种黄曲霉毒素(B1、B2、G1、G2和M1)的提取、分离、确证与定量方法。样品经80%(体积分数)的甲醇水溶液提取和免疫亲和固相萃取后,采用UHPLC-E S I/Q qQ-M S/M S的多反应监测模式实现分离、鉴定和外标法定量。5种目标毒素标准溶液的检出限(LOD)为0.05～0.3μg/L。在0.5～100μg/L的基质添加浓度范围内具有良好的线性关系(r2>0.99);以甘草为例,当添加水平为1.0μg/kg和5.0μg/kg时,得到62.3%～82.4%的回收率(相对标准偏差(RSD)<10%,n=6)。该方法灵敏度高、选择性和重复性好、回收率较高、检测速度快,适用于中成药及中药材等复杂基体中多种黄曲霉毒素的快速分析与筛查。
A method for the determination of five aflatoxins（B1,B2,G1,G2,M1） in Chinese patent medicines and medicinal herbs by immunoaffinity extraction coupled with ultra-high performance liquid chromatography-tandem mass spectrometry（UHPLC-MS/MS） was developed.The samples were extracted with 80%（v/v） methanol-water solution,followed by stepwise purification using an immunoaffinity column.The target compounds were then eluted with methanol.The extract was filtered then analyzed.With the gradient elution using a binary mobile phase containing of 0.1% formic acid-5 mmol/L ammonium acetate solution and methanol,the five aflatoxins were separated on an UHPLC BEH C18 column,followed by positive electrospray ionization and multi-reaction monitoring（MRM） provided by a triple-quadrupole tandem mass spectrometer.The limits of detection for the standard solution of aflatoxins ranged from 0.05-0.3 μg/L.The linear response was observed in the spiked concentration range of 0.5-100 μg/L with the correlation coefficients higher than 0.99.The spiked recoveries were within 62.3%-82.4% at the spiked levels of 1.0 μg/kg and 5.0 μg/kg for all the five aflatoxins with the relative standard deviations（RSDs） below 10%（n=6）.The developed method is sensitive,accurate,and reproducible with the reasonable recoveries,and can be applied to the determination of the 5 aflatoxins in the Chinese traditional patent medicines,medicinal herbs as well as other similar complex matrices.
出处
《色谱》
CAS
CSCD
北大核心
2011年第7期613-617,共5页
Chinese Journal of Chromatography
基金
北京市科委计划项目(D0805020031085)
关键词
免疫亲和萃取
超高效液相色谱-串联质谱
黄曲霉毒素
中成药
中药材
immunoaffinity extraction
ultra-high performance liquid chromatography-tandem mass spectrometry（UHPLC-MS/MS）
aflatoxins
Chinese patent medicines
medicinal herbs
