超高效液相色谱-串联质谱法同时测定小麦制品中4种交链孢霉毒素
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(1.北京市朝阳区疾病预防控制中心,北京 100021;2.北京市疾病预防控制中心 食物中毒诊断溯源技术北京市重点实验室,北京 100013)

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王硕 女 副主任技师 研究方向为理化检验 E-mail:serenashuo@163.com通信作者:┣┣(中)通信作者┫┫孙灵利 男 副研究员 研究方向为实验室管理E-mail:sheguansun@126.com

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Analysis of Alternaria in wheat products by ultra-high performance liquid chromatography-tandem mass spectrometry
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(1.Chaoyang District Center for Disease Control and Prevention,Beijing 100021,China;2.Beijing Key Laboratory of Diagnostic and Traceability Technologies for the Food Poisoning, Beijing Center for the Disease Control and Prevention, Beijing 100013, China)

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    摘要:

    目的 建立测定4种小麦制品(挂面、馒头、面包和饼干)中4种交链孢霉毒素的超高效液相色谱-串联质谱法。方法 4种小麦制品加入NaCl后,经酸化乙腈提取,固相萃取柱(SPE)净化后,以HSS T3色谱柱(2.1 mm×100 mm,1.7 μm)为分析柱,以0.15 mmol/L碳酸氢铵水溶液-甲醇为流动相进行梯度洗脱,以负离子电喷雾模式电离(ESI-),多反应离子监测(MRM)方式进行定性及定量检测,外标法定量。结果 在0.040~50 μg/L的线性范围内,4种交链孢霉毒素的回归方程均呈良好的线性关系,相关系数(r)>0.99。交链孢菌酮酸、交链孢酚、腾毒素和交链孢酚单甲醚的方法检出限分别为0.10、0.01、0.03和0.01 μg/kg,3个加标水平的回收率为85.7%~102%,相对标准偏差(RSD)为0.8%~11.0%。应用该方法对流通环节的挂面、馒头、面包和饼干进行检测,4种交链孢霉毒素均有检出,其浓度为0.02~185.00 μg/kg。结论 该方法灵敏度高、简便,适用于小麦制品中多种交链孢霉毒素的同时测定。

    Abstract:

    Objective To develop a method for determination of Alternaria in wheat products by ultra-high performance liquid chromatography-tandem mass spectrometry. Methods The samples were added NaCl and then extracted by acidized acetonitrile. The purification was carried out on a solid phase extraction (SPE). The separation was performed on an HSS T3 column(2.1 mm×100 mm,1.7 μm)using a mobile phase of 0.15 mmol/L ammonium bicarbonate aqueous solution-methanol by gradient elution. A multiple reaction monitoring (MRM) mode was employed in mass spectrometric detection. The matrix-matched external standard calibration was used for quantitation. Results Good linearities of the method were achieved over the concentration of 0.040-50 μg/L, with correlation coefficients above 0.99. The method detection limits (MDL) were 0.10,0.01,0.03 and 0.01 μg/kg for 4 kinds of Alternaria toxins. Average recoveries at three spiked levels were 85.7%-102% with relative standard deviations (RSD) of 0.8%-11.0%. The method was finally used to analyze Alternaria in wheat products and 4 target compounds were detected at a concentration range of 0.02-185.00 μg/kg. Conclusion This method could be applied in simultaneous analysis of Alternaria in wheat products.

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王硕,孙灵利,刘烨,安阳,张向明,邵兵.超高效液相色谱-串联质谱法同时测定小麦制品中4种交链孢霉毒素[J].中国食品卫生杂志,2019,31(1):35-40.

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  • 收稿日期:2019-01-09
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  • 在线发布日期: 2019-03-22
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