摘要
建立了快速准确测定蒸肉粉中6种真菌毒素含量的高效液相色谱-串联质谱(HPLC-MS/MS)方法。样品经水分散后用4%甲酸乙腈提取,氯化钠和硫酸镁盐析,以PriboFast MFC100多功能净化柱净化,Waters XBridge C_(18)色谱柱分离,电喷雾正离子(ESI+)模式电离,多反应监测(MRM)模式检测,基质匹配标准溶液外标法定量。结果表明,6种真菌毒素在0.1-10 ng/mL质量浓度范围内线性关系良好,相关系数(r)均>0.9995;6种目标物的方法检出限(LOD)均为0.1 μg/kg,方法定量限(LOQ)均为0.5 μg/kg;在3个加标水平(2.5、5 μg/kg和10 μg/kg)下平均回收率为84.9%-105.2%,相对标准偏差(RSD,n=6)为1.74%-6.02%。该方法具有成本低、快速、灵敏、准确、精密度高等优点,能满足蒸肉粉中真菌毒素残留的高通量检测。
A rapid and accurate analysis method based on high performance liquid chromatography coupled with triple quadrupole mass spectrometry (HPLC-MS/MS) was developed to screen and determine six mycotoxins in rice flour for steamed pork.The samples were dispersed by water,extracted with 4% formic acid acetonitrile,salted out with sodium chloride and magnesium sulphate.The extract was cleaned up with PriboFast MFC100 column.The target compounds were separated on a Waters XBridge C18 column,determined using electrospray ionization (ESI) source in positive mode with the multiple reaction monitoring (MRM) acquisition mode and quantified with the matrix-matched external standard method.Results showed that the 6 mycotoxins showed good linearity in their respective mass concentration ranges (0.1~10 ng/mL) with correlation coefficients (r) not less than 0.9995.The limits of detection (LOD) were 0.1 μg/kg,the limits of quantification (LOQ) were 0.5 μg/kg.At three spiked levels (2.5,5 μg/kg,and 10 μg/kg),the average recoveries for 6 target compounds were in the range of 84.9%~105.2% with relative standard deviations of 1.74%~6.02%.Therefore,the method is cheap,rapid,sensitive,accurate and high precision,and can be used for high-throughput detection of mycotoxins in rice flour for steamed pork samples.
作者
管卓龙
卢跃鹏
侯靖
许晴
田甜
王梦颖
杨明
涂凤琴
GUAN Zhuolong;LU Yuepeng;HOU Jing;XU Qing;TIAN Tian;WANG Mengying;YANG Ming;TU Fengqin(Wuhan Institute for Food and Cosmetic Control,Wuhan 430040,China)
出处
《食品科技》
CAS
北大核心
2021年第5期295-300,共6页
Food Science and Technology
基金
湖北省自然科学基金计划项目(2018CFB340)。
关键词
蒸肉粉
真菌毒素
高通量检测
高效液相色谱-串联质谱
rice flour for steamed pork
mycotoxin
high–throughput detection
high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)