全自动在线免疫亲和固相萃取-高效液相色谱法快速测定食品中的黄曲霉毒素
目的 建立一种全自动在线免疫亲和柱固相萃取-高效液相色谱(online immunoaffinity solid phase extraction-high performance liquid chromatography, online-IA-SPE-HPLC)快速测定食品中黄曲霉毒素(aflatoxins, AFT)。方法 样品经乙腈-水提取后, 经可重复使用的在线免疫亲和小柱进行富集与净化, 经C18色谱柱(150 mm×4.6 mm, 5 μm)进行分离, 用特定流动相进行洗脱, 用电化学衍生KOBRA?Cell荧光检测器进行检测, 激发波长为362 nm, 发射波长为455 nm, 同时进行线性范围、精密度、准确度和加标回收率等方法学验证。结果 对于大米、食醋、酱油和花生油等基质, 该方法对AFT B1的检出限均为0.035 μg/kg, 低于我国现行食品安全标准对AFT B1的限量要求; AFT B1及AFT G1在25~500 ng/L范围内具有良好的线性, AFT B2及AFT G2在6.25~125 ng/L范围内具有良好的线性, 相关系数均为0.9999; 在低、中和高3水平加标下大米、食醋、酱油和花生油中的4种黄曲霉毒素回收率在91.16%~109.99%之间, 精密度为0.52%~4.39%。结论 该方法的前处理快速、简易, 方法重现性好、灵敏度高, 适用于食品中AFT的高通量检测。
Objective To establish a method for rapid determination of total aflatoxins (AFT) in food by automated online immunoaffinity solid phase extraction- high performance liquid chromatography (online-IA-SPE- HPLC). Methods Samples were extracted with acetonitrile-water, further enriched and cleaned up with reusable online immunoaffinity solid phase. Aflatoxins were separated by a C18 reverse chromatographic column (150 mm×4.6 mm, 5 μm) with the proper mobile phase to flush and then detected by KOBRA?Cell fluorescence detector with excitation wavelength of 362 nm and emission wavelength of 455 nm. Furthermore, this established method was validated by linearity range, precision, accuracy and recovery. Results The results suggested that limits of determination (LOD) of AFT B1 was 0.035 μg/kg for food matrix including rice, vinegar, soy and peanut oil, which were lower than the maximum residue limit set by national standard. Good correlation coefficients (r2=0.9999) were obtained within the linear ranges of 25~500 ng/L for AFT B1 and AFT G1, 6.25~125 ng/L for AFT B2 and AFT G2, respectively. The recovery rates of 4 kinds of AFTs with low, intermediate and high spiking levels were 91.16%~109.99% with the precision of 0.52%~4.39% for all the matrix observed. Conclusion The proposed method is rapid, simple, repeatable and sensitive, which is suitable for high throughput determination of total aflatoxins in food.
标题：全自动在线免疫亲和固相萃取-高效液相色谱法快速测定食品中的黄曲霉毒素
英文标题：Rapid determination of aflatoxins in food by automated online immunoaffinity solid phase extraction-high performance liquid chromatography
作者：
曾羲 广州市食品检验所
蔡伟谊 广州市食品检验所
林子豪 广州市食品检验所
程军 拜发分析系统销售(北京)有限公司
戚平 广州市食品检验所
中文关键词:在线免疫亲和固相萃取,食品,黄曲霉毒素,液相色谱法,电化学衍生-荧光法,
英文关键词:online-immunoaffinity solid phase extraction,food,aflatoxins,liquid chromatography,electro chemistry derivative-fluorescence,
发表日期：2017-01-19
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