摘要
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B_(1)、B_(2)、G_(1)、G_(2)的标准曲线相关系数R^(2)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B、B_(2)、G_(1)、G_(2)进行抽检,其B_(1)、B_(2)检出率分别为4%、4%,G_(1)、G_(2)未检出。
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.Methods:The sample was extracted with acetonitrile-water(volume ratio 70:30),centrifuged,and the supernatant was diluted with phosphate buffer 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 R^(2)of aflatoxin B_(1),B_(2),G_(1),and G_(2)are 0.9986,0.9996,0.9984,and 0.9970 respectively;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 spectrometry method is simple,rapid,highly sensitive and precise,and can meet the needs of determining aflatoxin content in large batches of traditional Chinese medicine pieces of astragalus and a reference method for the detection of other Chinese medicinal materials.Using this method,aflatoxin B_(1),B_(2),G_(1)and G_(2)in 50 pieces of traditional Chinese medicine pieces of astragalus were sampled.The detection rates of Br and B_(2)were 4%and 4%respectively,while G_(1)and G_(2)were not detected.
作者
陈旭
刘春波
李桂平
CHEN Xu;LIU Chunbo;LI Guiping(Inner Mongolia Autonomous Region Hospital of Traditional Chinese Medicine,Hohhot,Inner Mongolia 010010;Hohhot City Center for Disease Control and Prevention,Hohhot,Inner Mongolia 010010)
出处
《内蒙古中医药》
2024年第11期143-145,168,共4页
Inner Mongolia Journal of Traditional Chinese Medicine
