化学工程师Sum335No.8ChemicalEngineerDO1:10.16247/j.cnki.23-1171/tq.20230834分析测试2023年第8期地龙药材中黄曲霉毒素B1、B2、GI、G2的含量检测*李正刚1,程焱1,王丹或1,赵艳²,马或1(1.四平市食品药品检验所,吉林四平1360002.吉林省药品检验研究院,吉林长春130000)摘要:目的建立超声萃取-免疫亲和柱净化-柱后光化学衍生法高效液相色谱法同时测定地龙药材中黄曲霉毒素B1、B2、G1、G2含量的测定方法。方法样品粉碎过120目筛后,采用70%甲醇超声处理30min,经免疫亲和柱净化、高效液相色谱分离、光化学柱后衍生,通过荧光检测器测定4种黄曲霉毒素的含量。结果线性范分别为:黄曲霉毒素B:0.0104~0.0520ng(r=0.9999)黄曲霉毒素B20.0038~0.0190ng(r=0.9998)、黄曲霉毒素Gl0.0108~0.0540ng(r=0.9998)、黄曲霉毒素G20.0038~0.0190ng(r=0.9998),线性关系良好。检出限分别为0.43、0.15、0.43、0.15μg°kg。回收率在90.42~99.47%之间,RSD≤3.2%(n=6)。结论该方法操作简便,灵敏度高、重复性好、结果准确,可用于地龙中黄曲霉毒素含量的测定。关键词:超声提取;免疫亲和柱;光化学衍生;黄曲霉毒素;地龙中图分类号:R286.0LIZheng-gang',CHENGYan',WANGDan-yu',zZHAOYan²,MAYui(1.SipingInstituteforFoodandDrugControl,Siping13600,Chinai2.jilinInstitutesforDrugControl,Changchun130000,China)Abstract:OBJECTIVEToestablishHPLCmethodforthesimultaneousdeterminationofaflatoxinBi,B2,GiandG2inPheretimabyultrasonicextraction-immunoaffinitycolumnclean-upandpost-columnphotochemicalderivatization.METHODThesamplewascrushedandpassedthrougha120-meshsieveandextractedwith70%methanolfortiirtyminutesandpurificationbyimmunoaffinitycolumns,aflatoxinBi,B2,GiandG,insampleswereanlyzedbyHPLC-FLDwithpost-columnphotochemicalderivatization.RESULTSThelinearityofaflatoxinBiwasat0.0104~0.0520ng(r=0.9999),aflatoxinB2wasat0.0038~0.0190ng(r=0.9998),AflatoxinGiwasat0.0108~0.0540ng(r=0.9998),AflatoxinG2wasat0.0038~0.0190ng(r=0.9998),thedetectionlimitswere0.43、0.15、0.43.0.15μgkg-,respectively.Therecoveriesrangedfrom90.42%to99.47%withtheRSD≤3.2%(n=6).CONCLUSIONThemethodissimple,sensitive,reproducibleandaccurate,ThismethodissuitableforthedeterminationofAFinPheretima,Keywords:ultra...