柱后碘衍生—高效液相色谱法测定脂必妥片中黄曲霉毒素B1的含量  

Determination for Content of Aflatoxins B1 in Zhibituo Tablet by RP-HPLC with Iodine Derivative

作　　者：罗霄 代琪 曾桢 汪丹[2,3] 

机构地区：[1]成都市食品药品检验研究院,四川成都6101061 [2]成都大学基础医学与护理学院,四川成都610106 [3]四川大学华西药学院,四川成都610041

出　　处：《成都大学学报（自然科学版）》2015年第3期238-239,254,共3页Journal of Chengdu University（Natural Science Edition）

摘　　要：为建立测定脂必妥片中黄曲霉毒素B1含量的高效液相分析法,样品经80%甲醇溶液超声提取后,通过免疫亲合柱净化、柱后碘衍生化,以荧光检测器检测,采用Waters Sunfire C18色谱柱（4.6 mm×250 mm,5μm）;甲醇—乙腈—水（40∶18∶42）为流动相;流速,0.8 m L/min;柱温,25℃;衍生溶液为0.05%的碘溶液,衍生化泵流速,0.3 m L/min,衍生化温度70℃;激发波长λex=360 nm,发射波长λem=450 nm.结果显示,黄曲霉毒素B1在0.0008~0.0040 ng（r=0.9999）范围内呈良好的线性关系;回收率为97.13%（RSD=0.73%）,检出限为0.5μg/kg.本方法简便,结果准确可靠,适于测定脂必妥片中黄曲霉毒素B1的含量.The paper establishes an analytical method to test the content of Aflatoxins B1 in Zhibituo Tablet by RP-HPLC. Firstly, the sample Aflatoxins B1 is extracted with 80% MeOH, and then it is purified by immunoaffinity columns and finally, the sample will be tested by fluorescence detector. The Waters Sunfire C 18 chromatographic column （4.6× 250 mm, 5μm ） column and methanol-acetonitrile-water （ 40： 18 ： 42） as a mobile phase are used at 25℃ with a flow rate of 0.8 mL/min. The pest-derivatization solution is iodine solution of 0.05%, and the post-derivatization flow is 0.3 mL/min with a derivatization temperature of 70℃ by the excitation wavelength of 360 nm and emission wavelength of 450 nm. Aflatoxins B1 presents a good linear correlation in range of 0.0008 - 0.0040 ng（r = 0.9999）. The average recovery rate is 97.13 % （RSD = 0.73 % ）. The detection limit of the method is 0.5 μg/kg. This method is convenient and reliable, and is suitable for the detection of aflatoxins B1 in Zhibituo Tablet.

关 键 词：脂必妥片 黄曲霉毒素B1 柱后衍生法 免疫亲和柱 

分 类 号：R927[医药卫生—药学]