固相萃取-超高效液相色谱-串联质谱法检测猪肉中玉米赤霉醇类的残留量

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1.0~100 μ g/L,相关系数大于0.999;各化合物在组织中的检出限为0.03~0.09 μ g/kg;样品在1.0~10.0 μ g/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。

Determination of zearalanol and related mycotoxins in pork by solid-phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry

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 μ g/L based on the internal standard calibration. The detection limits of the method were 0.03-0.09 μ g/kg. The mean recoveries of the six target compounds spiked at three levels from 1.0-10.0 μ g/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.