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

doi:10.7506/spkx1002-6630-201724047

食品科学 ›› 2017, Vol. 38 ›› Issue (24): 288-295.doi: 10.7506/spkx1002-6630-201724047

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

周健，许娇娇，金米聪，蔡增轩，黄百芬，任一平

（1.浙江省疾病预防控制中心理化毒理所，浙江?杭州 310051；2.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，浙江?宁波 315010；3.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，浙江?嘉兴 314006）

收稿日期:2017-12-07 修回日期:2017-12-07 出版日期:2017-12-25 发布日期:2017-12-07

Optimization and Validation of QuEChERS Extraction for Determination of Sterigmatocystin in Eggs by Response Surface Methodology

ZHOU Jian, XU Jiaojiao, JIN Micong, CAI Zengxuan, HUANG Baifen, REN Yiping

(1. Department of Physicochemical & Toxicology, Zhejiang Provincial Centre for Disease Control and Prevention, Hangzhou 310051, China; 2. Zhejiang Provincial Key Lab of Health Risk Appraisal for Trace Toxic Chemicals, Ningbo Municipal Centre for Disease Control and Prevention, Ningbo 315010, China; 3. Zhejiang Yangtze Delta Region Institute of Tsinghua University, Application Technology Cooperation Center of National Center for Food Safety Risk Assessment, Jiaxing 314006, China)

Received:2017-12-07 Revised:2017-12-07 Online:2017-12-25 Published:2017-12-07

摘要/Abstract

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Na2SO4、NaCl和无水CH3COONa进行盐析，取出上层乙腈后加入C18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0.1?μg/kg，定量限为0.5?μg/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?608?μg/kg。

关键词: 鸡蛋, 杂色曲霉毒素, QuEChERS法, 响应面法, 超高效液相色谱-质谱联用

Abstract: A quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction procedure was presented andoptimized for the determination of sterigmatocystin in eggs by high performance liquid chromatography-mass spectrometry (HPLC-MS). The analyte was extracted from samples with aqueous acetonitrile solution, followed by salting out using anhydrous NaSO4, NaCl and CH3COONa,and then purification and concentration with C18 sorbent and anhydrous Na2SO4 before analysis. Optimization of experimental conditions for maximum extraction efficiency was carried out using Plackett-Burman design, one-factor-at-a-time method and response surface methodology. The matrix-matched external standard calibration was employed for quantification. Moreover, all positive sampleswere confirmed by immunoaffinity column chromatography. The results of validation showed that good linearity with a correlation coefficient (R2) > 0.999 6 was achieved within the range from 0.125 to 1 000 ng/mL. The limit of detection (LOD) and the limit of quantification (LOQ) for sterigmatocystin in eggs were 0.1 and 0.5 μg/kg, respectively. Satisfactory recovery (86.8%–90.4%) and inter-day reproducibility (RSD, 1.5%–6.2%) were obtained with blank egg matrices at three spiked levels. Finally, the established method was applied to analyze 45 real samples, 10 of which were positive at concentrations of 0.5 to 3 608 μg/kg.

Key words: egg, sterigmatocystin, QuEChERS extraction, response surface methodology, high performance liquid chromatography-mass spectrometry

中图分类号:

O657.63

周健，许娇娇，金米聪，蔡增轩，黄百芬，任一平. 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[J]. 食品科学, 2017, 38(24): 288-295.

ZHOU Jian, XU Jiaojiao, JIN Micong, CAI Zengxuan, HUANG Baifen, REN Yiping. Optimization and Validation of QuEChERS Extraction for Determination of Sterigmatocystin in Eggs by Response Surface Methodology[J]. FOOD SCIENCE, 2017, 38(24): 288-295.

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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

Optimization and Validation of QuEChERS Extraction for Determination of Sterigmatocystin in Eggs by Response Surface Methodology

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