利用超高效液相色谱-串联质谱(UPLC-MS/MS)结合同位素稀释技术测定了猪肉食品中6种玉米赤霉醇类物质.猪肉样品经β-葡萄糖苷酶/硫酸酯酶水解,甲醇水溶液提取,HLB固相萃取柱富集净化后,以纯水和乙腈为流动相在BEH C18反相柱上分离,采用电喷雾电离源负离子模式(ESI-)在多反应监测模式(MRM)模式下进行扫描.以2种经氘代同位素标记的玉米赤霉烯醇为内标进行定量.猪肉中6种目标物的线性范围为1.0～100μg/L,相关系数大于0.999;各化合物在组织中的检出限为0.03 ～0.09μg/kg;样品在1.0～10.0 μg/kg的加标回收率为76.7％ ～ 100.5％,相对标准偏差不大于20％.该方法具有操作简单,灵敏度高,重现性好等特点,符合食品样品中痕量污染物的检测要求.%A method was established for the determination of six compounds of zearalanol and related mycotoxins in pork and its products.After hydrolysis of the target compounds in the pork by β-glucosidase/sulfatase,they were extracted with methanol aqueous solution and further purified by an HLB column.The separation was performed on a BEH C18 column with gradient elution using acetonitrile-water as mobile phases.The analytes were determined by mass spectrometry using electrospray ionization (ESI) in negative scan mode and multiple reaction monitoring (MRM) mode.α-Zearalenol-D7 and β-zearalenol-D7 were used as internal standards.The good linearities (r ＞ 0.999) were achieved for the six compounds over the range of 1.0-100 μg/L based on the internal standard calibration.The detection limits of the method were 0.03-0.09 μg/kg.The mean recoveries of the six target compounds spiked at three levels from 1.0-10.0 μg/kg ranged from 76.7％ to 100.5％ with the relative standard deviations (RSDs) less than 20％.The proposed method is simple,sensitive,reproducible,and complies with the regulations for the determination of trace contaminant residues in food matrices.
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