柱后光化学衍生高效液相色谱法同时测定调味品中黄曲霉毒素M1.docVIP

柱后光化学衍生高效液相色谱法测定调味品中黄曲霉毒素 王韦岗 唐双双 陆源 朱新生 （镇江市产品质量监督检验所，江苏镇江 212132） 摘要：建立了高效液相色谱法同时测定调味品中黄曲霉毒素B1、B2、G1、G2和M1的方法。用乙腈和水的混合溶液（体积比为80：20）提取样品中五种黄曲霉毒素，提取液经中性氧化铝固相萃取柱和Mycosep 228 AflaPat多功能净化柱净化，采用C18色谱柱分离，光化学衍生后进入荧光检测器测定，外标法定量。黄曲霉毒素B1、B2、G1、G2和M1的最低检出限分别为0.50μg/kg、0.10μg/kg、0.50μg/kg、0.10μg/kg和0.50μg/kg，对四种调味品进行加标回收和精密度实验，回收率均在85%以上，相对标准偏差（RSD）为1.27%~4.82%。实验结果表明，该方法操作简单，速度快，重现性好，满足调味品中黄曲霉毒素检测的要求。 关键词：固相萃取；多功能净化柱；光化学衍生；黄曲霉毒素；调味品 Determination of aflatoxins in Condiment by HPLC with post-column photochemical derivatization Wang Wei-gang，Tang Shuang-shuang，Lu Yuan，Zhu Xin-sheng (Zhenjiang Institute for Products Quality Supervision and Inspection, Zhenjiang 212009, China；) Abstract：To develop a high performance liquid chromatography with post-column derivatization method for simultaneous determination of Aflatoxins B1、B2、G1、G2、M1. The five kinds of Aflatoxins in samples were extracted by acetonitrile/water(80:20,V/V). The extract was purified by solid phase extraction column and Mycosep 228 AflaPat multifunctional clean-up column，separated with C18 chromatographic column. The toxins were detected by fluorescence detector after photochemical derivatization , and quantitatived by external standard method. The detection limits of Aflatoxin B1、B2、G1、G2 and M1 were 0.50μg/kg、0.10μg/kg、0.50μg/kg、0.10μg/kg and 0.50μg/kg respectively，the results of recovery and precision experiment showed that the recovery were above 85%, the relative standard deviation RSD(%) were 1.27%~4.82%. The results show that the method is simple, faster, good repeatability and more suited to the requirements of Aflatoxins testing in condiment. Key words: Solid phase extraction；Multifuntional clean-up column; Photochemical derivatization; Aflatoxin; Condiment -------------------------------------- 通讯作者：王韦岗，硕士，研究方向：主要从事食品检验和研究工作，Tel E-mail：weigang228@163.com 黄曲霉毒素是黄曲霉和寄生曲霉的代谢产物，是一种常见的腐生真菌，多见于发霉的粮食、粮食制品及其他霉腐的有机物上，主要存在形式为B1、B2、G1、G2、M1和M2。在天然污染的食品中以黄曲霉毒素B1最为常见，其毒性和致癌性也是最强。1993年黄曲霉毒素被世界卫生组织(WHO