首页|中药黄芪饮片中黄曲霉毒素B1、B2、G1、G2的UPLC-MS/MS分析测定

中药黄芪饮片中黄曲霉毒素B1、B2、G1、G2的UPLC-MS/MS分析测定

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目的:通过超高效液相色谱-串联质谱法建立对中药黄芪饮片中黄曲霉毒素的含量的测定,了解中药黄芪饮片的质量安全状况.方法:样品经乙腈-水(体积比70∶30)提取、离心后得到的上清液用磷酸盐缓冲溶液稀释后通过免疫亲和柱净化和富集,洗脱液过滤后,经优化流动相后反相色谱分离,串联质谱检测,内标法定量.结果:采用5mmoL/L甲酸铵溶液(含0.1%甲酸)和乙腈∶甲醇=1∶1(含0.1%甲酸)作流动相时,黄曲霉毒素B1、B2、G1、G2的标准曲线相关系数R2分别是0.9986、0.9996、0.9984、0.9970;其加标回收率分别为105%、95.4%、107%、98.8%;RSD在2.46%~4.90%;其方法检出限为0.06ug/kg,定量限为0.20ug/kg.结论:超高效液相色谱-串联质谱法简单快速,灵敏度高,精密度高,可满足大批量中药黄芪饮片中黄曲霉毒素含量测定的需要以及对其它中药材的检测参考方法;利用此法对50份中药黄芪饮片中黄曲霉毒素B1、B2、G1、G2进行抽检,其B1、B2检出率分别为4%、4%,G,、G2未检出.
Determination of Aflatoxin B1,B2,G1 and G2 in Radix Astragali Pieces by UPLC-MS/MS
Objective:To establish an ultra-performance liquid chromatography-tandem mass spectrometry method for the determination of aflatoxin content in Radix Astragali decoction pieces,and understand the quality and safety status of Radix Astragali decoction pieces.Meth-ods:The sample was extracted with acetonitrile-water(volume ratio 70∶30),centrifuged,and the supernatant was diluted with phosphate buf-fer solution,purified and enriched by immunoaffinity column.After the eluent was filtered,it was separated by reverse phase chromatography after optimized mobile phase,detected by tandem mass spectrometry,and quantified by internal standard method.Results:Use 5mmoL/L ammonium formate solution(containing 0.1%formic acid)and acetonitrile∶methanol=1∶1 When(containing 0.1%formic acid)is used as the mobile phase,the standard curve correlation coefficients R2 of aflatoxin B1,B2,G1,and G2 are 0.9986,0.9996,0.9984,and 0.9970 respective-ly;the spiked recoveries are 105%,95.4%,107%,and 98.8%respectively;the RSD is 2.46%~4.90%;the method limit of detection is 0.06ug/kg,and the limit of quantification is 0.20ug/kg.Conclusion:The ultra-performance liquid chromatography-tandem mass spectrome-try method is simple,rapid,highly sensitive and precise,and can meet the needs of determining aflatoxin content in large batches of tradi-tional Chinese medicine pieces of astragalus and a reference method for the detection of other Chinese medicinal materials.Using this meth-od,aflatoxin B1,B2,G1,and G2 in 50 pieces of traditional Chinese medicine pieces of astragalus were sampled.The detection rates of B1 and B2 were 4%and 4%respectively,while G1 and G2were not detected.

Ultra-performance liquid chromatography-tandem mass spectrometryImmunoaffinity columnAflatoxin B1,B2,G1,G2

陈旭、刘春波、李桂平

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内蒙古自治区中医医院 内蒙古 呼和浩特 010010

呼和浩特市疾病预防控制中心 内蒙古 呼和浩特 010010

超高效液相色谱-串联质谱 免疫亲和柱 黄曲霉毒素B,、B2、G,、G2

2024

内蒙古中医药
内蒙古自治区中医药学会,内蒙古自治区中蒙医研究所

内蒙古中医药

影响因子:0.444
ISSN:1006-0979
年,卷(期):2024.43(11)