QuEChERS-超高效液相色谱-串联质谱法同时测定畜禽组织中6种黄曲霉毒素和杂色曲霉素

引用本文: 凌阿茹, 郭文博, 杨俊花, 赵志辉, 郭晋丽. QuEChERS-超高效液相色谱-串联质谱法同时测定畜禽组织中6种黄曲霉毒素和杂色曲霉素[J]. 色谱, 2018, 36(5): 439-445. doi: 10.3724/SP.J.1123.2017.11028 shu

Citation: LING Aru, GUO Wenbo, YANG Junhua, ZHAO Zhihui, GUO Jinli. Simultaneous determination of six aflatoxins and sterigmatocystin in livestock and poultry tissues by QuEChERS-ultra high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2018, 36(5): 439-445. doi: 10.3724/SP.J.1123.2017.11028 shu

QuEChERS-超高效液相色谱-串联质谱法同时测定畜禽组织中6种黄曲霉毒素和杂色曲霉素

上海市农业科学院农产品质量标准与检测技术研究所, 上海 201403
基金项目:
上海市自然科学基金（17ZR1418800）；上海市农委科技兴农重点攻关项目（沪农科攻字（2013）第3-8号）.

摘要: 建立了QuEChERS前处理技术结合超高效液相色谱-串联质谱（UHPLC-MS/MS）检测畜禽组织中6种黄曲霉毒素和杂色曲霉素残留的分析方法。样品经20 μL β-葡萄糖苷酶酶解和10 mL乙腈-水（84：16，v/v）提取，然后用1.0 g氯化钠和1.0 g无水硫酸镁净化、5 mL正己烷脱脂，最后采用1 mL含5 mmol/L乙酸铵的乙腈-水溶液（80：20，v/v）复溶。以甲醇和5 mmol/L乙酸铵为流动相，在多反应监测正离子模式下进行检测，采用基质匹配标准曲线外标法进行定量分析。结果显示，6种黄曲霉毒素和杂色曲霉素在各自的范围内线性关系良好，相关系数（R²）>0.99，检出限（LOD，S/N=3）为0.007~0.30 μg/kg，定量限（LOQ，S/N=10）为0.02~0.91 μg/kg，加标回收率为77.3%~118.5%（n=6）。该法简单、快速，灵敏度高，适用于不同畜禽产品中6种黄曲霉毒素和杂色曲霉素的确证分析。

关键词:

English

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

Institute for Agri-Food Standards and Technology, Shanghai Academy of Agricultural Sciences, Shanghai 201403, China
Received Date: 22 November 2017
Fund Project:
Shanghai Natural Science Foundation (No. 17ZR1418800)

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 (R²) were greater than 0.99. The limits of detection (LODs, S/N=3) and the limits of quantification (LOQs, S/N=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.

Key words:

ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS)
/ QuEChERS
/ aflatoxins (AFTs)
/ sterigmatocystin (SMC)
/ livestock and poultry tissues

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QuEChERS-超高效液相色谱-串联质谱法同时测定畜禽组织中6种黄曲霉毒素和杂色曲霉素

English

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

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

QuEChERS-超高效液相色谱-串联质谱法同时测定畜禽组织中6种黄曲霉毒素和杂色曲霉素

English

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

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

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CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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通讯作者: 陈斌, bchen63@163.com

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