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[基于QuEChERS-超高效液相色谱-串联质谱法同时测定畜禽组织中的六种黄曲霉毒素和杂色曲霉素]

[Simultaneous determination of six aflatoxins and sterigmatocystin in livestock and poultry tissues by QuEChERS-ultra high performance liquid chromatography-tandem mass spectrometry].

作者信息

Ling Aru, Guo Wenbo, Yang Junhua, Zhao Zhihui, Guo Jinli

机构信息

Institute for Agri-Food Standards and Technology, Shanghai Academy of Agricultural Sciences, Shanghai 201403, China.

出版信息

Se Pu. 2018 May 8;36(5):439-445. doi: 10.3724/SP.J.1123.2017.11028.

DOI:10.3724/SP.J.1123.2017.11028
PMID:30136484
Abstract

A method for the simultaneous determination of six aflatoxins (AFTs) and sterigmatocystin (SMC) in livestock and poultry tissues by QuEChERS-ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was developed and validated. The samples were extracted with 10 mL acetonitrile-water (84:16, v/v) after enzymatic hydrolysis with 20 μL β-glucosidase. The extracts were cleaned with 1.0 g each of sodium chloride and anhydrous magnesium sulfate, and then degreased with 5 mL hexane. The residues were re-dissolved in 1 mL acetonitrile-water (80:20, v/v) containing 5 mmol/L ammonium acetate. Methanol and 5 mmol/L ammonium acetate were used as the mobile phases. Six AFTs and SMC were analyzed by multiple reaction monitoring in the positive ion mode. Matrix-matched calibration curves and external standards were used for the accurate quantification of the six AFTs and SMC. Good linear relationships were obtained, the correlation coefficients () were greater than 0.99. The limits of detection (LODs, =3) and the limits of quantification (LOQs, =10) ranged from 0.007 to 0.30 μg/kg, and 0.02 to 0.91 μg/kg, respectively. The recoveries at different spiked levels were satisfactory, and ranged from 77.3% to 118.5%. This method is simple, easy and sensitive, and is suitable for the rapid determination of the six AFTs and SMC in different pork, pork liver and chicken samples.

摘要

建立并验证了一种采用QuEChERS-超高效液相色谱-串联质谱法(UHPLC-MS/MS)同时测定畜禽组织中6种黄曲霉毒素(AFTs)和杂色曲霉素(SMC)的方法。样品经20 μL β-葡萄糖苷酶酶解后,用10 mL乙腈-水(84:16,v/v)提取。提取物用1.0 g氯化钠和无水硫酸镁净化,然后用5 mL正己烷脱脂。残渣重新溶解于1 mL含5 mmol/L乙酸铵的乙腈-水(80:20,v/v)中。以甲醇和5 mmol/L乙酸铵为流动相。采用多反应监测正离子模式分析6种AFTs和SMC。采用基质匹配校准曲线和外标法对六种AFTs和SMC进行准确定量。获得了良好线性关系,相关系数()大于0.99。检测限(LODs,=3)和定量限(LOQs,=10)分别为0.0070.30 μg/kg和0.020.91 μg/kg。不同加标水平下的回收率令人满意,范围为77.3%至118.5%。该方法简便、灵敏,适用于不同猪肉、猪肝和鸡肉样品中6种AFTs和SMC的快速测定。

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