色谱

色谱 ›› 2018, Vol. 36 ›› Issue (5): 439-445.DOI: 10.3724/SP.J.1123.2017.11028

• 研究论文 • 上一篇    下一篇

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

凌阿茹, 郭文博, 杨俊花, 赵志辉, 郭晋丽   

  1. 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
  • 收稿日期:2017-11-22 出版日期:2018-05-08 发布日期:2014-03-21
  • 通讯作者: 杨俊花.Tel:(021)67131637,E-mal:yangjunhua303@126.com
  • 基金资助:

    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）.

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

LING Aru, GUO Wenbo, YANG Junhua, ZHAO Zhihui, GUO Jinli   

  1. Institute for Agri-Food Standards and Technology, Shanghai Academy of Agricultural Sciences, Shanghai 201403, China
  • Received:2017-11-22 Online:2018-05-08 Published:2014-03-21
  • Supported by:

    Shanghai Natural Science Foundation (No. 17ZR1418800); Developing Agriculture Key Project through Science and Technology of Shanghai Agricultural Commission (Agricultural Attack Word 2013-3-8).

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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: QuEChERS, 超高效液相色谱-串联质谱, 黄曲霉毒素, 畜禽组织, 杂色曲霉素

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

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