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,1.7μm)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0.040～50μg/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0.01μg/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0.02～185.00μg/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。
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.
作者
王硕
孙灵利
刘烨
安阳
张向明
邵兵
WANG Shuo;SUN Lingli;LIU Ye;AN Yang;ZHANG Xiangming;SHAO Bing(Chaoyang District Center for Disease Control and Prevention,Beijing 100021,China;Beijing Key Laboratory of Diagnostic and Traceability Technologies for the Food Poisoning,Beijing Center for the Disease Control and Prevention,Beijing 100013,China)
出处
《中国食品卫生杂志》
CSCD
北大核心
2019年第1期35-40,共6页
Chinese Journal of Food Hygiene
关键词
交链孢霉毒素
小麦制品
超高效液相色谱-串联质谱
霉菌毒素
食品污染物
Alternaria toxins
wheat products
ultra-high performance liquid chromatography-tandem mass spectrometry
mycotoxin
food contaminants
