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

色谱 , 2013, 31(7): 703-708. doi: 10.3724/SP.J.1123.2012.12033

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

李丽萍 ^1, , 范赛 ^2, , 赵榕 ^3, , 李兵 ^4, , 刘伟 ^5, , 吴国华 ^6,

1.北京市疾病预防控制中心营养与食品卫生所,北京,100013

2.北京市疾病预防控制中心营养与食品卫生所,北京,100013

3.北京市疾病预防控制中心营养与食品卫生所,北京,100013

4.北京市疾病预防控制中心营养与食品卫生所,北京,100013

5.北京市疾病预防控制中心营养与食品卫生所,北京,100013

6.北京市疾病预防控制中心营养与食品卫生所,北京,100013

基金项目: 北京市自然科学基金项目(7102087)

关键词：固相萃取 , 超高效液相色谱-串联质谱 , 玉米赤霉醇 , 真菌毒素

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

Keywords： solid-phase extraction (SPE) , ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) , zearalanol , mycotoxin

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.

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