响应面试验优化QuEChERS法提取鸡蛋中杂色曲霉毒素工艺及方法学验证

发布时间：2018-04-23 20:00

本文选题：鸡蛋 + 杂色曲霉毒素　；参考：《食品科学》2017年24期

【摘要】：使用乙腈溶液对鸡蛋中杂色曲霉毒素进行提取,后加入无水Na_2SO_4、NaCl和无水CH_3COONa进行盐析,取出上层乙腈后加入C_(18)吸附剂和无水Na2SO4进行净化浓缩后上机检测。采用Plackett-Burman试验、单因素试验和响应面法优化,最大限度地提高杂色曲霉毒素的提取率。使用基质匹配曲线外标法定量,所有阳性样品均使用免疫亲和柱法复测。结果表明,杂色曲霉毒素在0.125~1 000 ng/mL质量浓度范围内线性良好,相关系数达0.999 6,检出限为0.1μg/kg,定量限为0.5μg/kg。在空白鸡蛋基质中进行三水平加标实验,测得提取率在86.8%~90.4%范围内,日间重复性在1.5%~6.2%范围内。最终,将建立的方法用于45份样品检测,其中10份鸡蛋样品检测结果呈阳性,含量为0.5~3 608μg/kg。
[Abstract]:Aspergillus mutans was extracted from eggs with acetonitrile solution, then added anhydrous Na2SO4Na2SO4NaCl and anhydrous CH_3COONa to salting-out. The top acetonitrile was removed and then added CTA18) adsorbent and anhydrous Na2SO4 were used for purification and concentration. Plackett-Burman test, single factor test and response surface method were used to optimize the extraction rate of aspergillus mutans. All positive samples were determined by immunoaffinity column method. The results showed that the calibration curve of aspergillus mutans was linear in the concentration range of 0.125 ~ 1 000 ng/mL, the correlation coefficient was 0.999, the detection limit was 0.1 渭 g / kg, and the quantitative limit was 0.5 渭 g / kg. The results showed that the extraction rate was in the range of 86.8% and the daily repeatability was in the range of 1.5% and 6.2% respectively. Finally, the established method was used to detect 45 samples, 10 of which were positive, and the content of egg samples was 0.53608 渭 g / kg 路kg ~ (-1) 路kg ~ (-1) ~ (-1) ~ (-1) ~ (-1) ~ (-1).
【作者单位】：浙江省疾病预防控制中心理化毒理所;宁波市疾病预防控制中心浙江省微量有毒化学物健康风险评估技术研究重点实验室;国家食品安全风险评估中心应用技术合作中心浙江清华长三角研究院;
【分类号】：O657.63;TS253.4

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