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猪肉、猪肝中盐酸克伦特罗、莱克多巴胺、特布他林及沙丁醇胺的检测本文就瘦肉精(克伦特罗、莱克多巴胺、特布他林及沙丁醇胺)扩项认证实验方法的确认过程进行详细解读。涉及的标准:[img=,690,84]http://ng1.17img.cn/bbsfiles/images/2018/08/201808162144287540_8130_2166779_3.png!w690x84.jpg[/img]液相色谱条件:[img=,690,311]http://ng1.17img.cn/bbsfiles/images/2018/08/201808162142182407_2039_2166779_3.png!w690x311.jpg[/img]MRM质谱条件:[img=,656,332]http://ng1.17img.cn/bbsfiles/images/2018/08/201808162143190310_6780_2166779_3.png!w656x332.jpg[/img]盐酸克伦特罗、莱克多巴胺、特布他林及沙丁醇胺均为5ng/mL(含内标物)的TIC图及MRM图:[img=,649,449]http://ng1.17img.cn/bbsfiles/images/2018/08/201808162209329386_2102_2166779_3.png!w649x449.jpg[/img]其中克伦物罗只采集277.2>132、277.2>202.9这两个子离子:[img=,690,219]http://ng1.17img.cn/bbsfiles/images/2018/08/201808162210045860_1385_2166779_3.png!w690x219.jpg[/img][img=,656,206]http://ng1.17img.cn/bbsfiles/images/2018/08/201808162211276827_3238_2166779_3.png!w656x206.jpg[/img][img=,690,397]http://ng1.17img.cn/bbsfiles/images/2018/08/201808162213301990_3525_2166779_3.png!w690x397.jpg[/img][img=,690,412]http://ng1.17img.cn/bbsfiles/images/2018/08/201808162213400460_418_2166779_3.png!w690x412.jpg[/img]猪肉样品的测定结果:[img=,690,458]http://ng1.17img.cn/bbsfiles/images/2018/08/201808162218508377_830_2166779_3.png!w690x458.jpg[/img][img=,678,221]http://ng1.17img.cn/bbsfiles/images/2018/08/201808162219077610_3828_2166779_3.png!w678x221.jpg[/img][img=,690,435]http://ng1.17img.cn/bbsfiles/images/2018/08/201808162219185997_7107_2166779_3.png!w690x435.jpg[/img][img=,690,423]http://ng1.17img.cn/bbsfiles/images/2018/08/201808162219325567_679_2166779_3.png!w690x423.jpg[/img]在猪肉基质中的检测限:0.1ng/mL克伦特罗:[img=,690,526]http://ng1.17img.cn/bbsfiles/images/2018/08/201808162223406730_6485_2166779_3.png!w690x526.jpg[/img]0.5ng/mL莱克多巴胺:[img=,690,521]http://ng1.17img.cn/bbsfiles/images/2018/08/201808162226394828_9955_2166779_3.png!w690x521.jpg[/img]0.5ng/mL沙丁醇胺:[img=,690,405]http://ng1.17img.cn/bbsfiles/images/2018/08/201808162228398089_6245_2166779_3.png!w690x405.jpg[/img]0.5ng/mL特布他林:[img=,690,506]http://ng1.17img.cn/bbsfiles/images/2018/08/201808162233035297_131_2166779_3.png!w690x506.jpg[/img]克伦特罗、莱克多巴胺、沙丁醇胺、特布他林的检出限及工作曲线方程及相关系数:[img=,690,333]http://ng1.17img.cn/bbsfiles/images/2018/08/201808162233124587_911_2166779_3.png!w690x333.jpg[/img]猪肉样品加标回收:[img=,690,81]http://ng1.17img.cn/bbsfiles/images/2018/08/201808162242399324_8197_2166779_3.png!w690x81.jpg[/img][img=,690,595]http://ng1.17img.cn/bbsfiles/images/2018/08/201808162245573160_5901_2166779_3.png!w690x595.jpg[/img][img=,690,464]http://ng1.17img.cn/bbsfiles/images/2018/08/201808162246112180_6133_2166779_3.png!w690x464.jpg[/img][img=,642,359]http://ng1.17img.cn/bbsfiles/images/2018/08/201808162246257140_8429_2166779_3.png!w642x359.jpg[/img]鸡肝样品中的克伦特罗如果只采集277.2>132、277.2>202.9这两个子离子出现了假阳性:代入工作曲线得鸡肝样品中的克伦特罗为4ug/kg,不合格啊??[img=,690,388]http://ng1.17img.cn/bbsfiles/images/2018/08/201808162256222427_6524_2166779_3.jpg!w690x388.jpg[/img]样品与标液重叠图谱克伦特罗:[img=,690,388]http://ng1.17img.cn/bbsfiles/images/2018/08/201808162259258447_6528_2166779_3.jpg!w690x388.jpg[/img]结合好几个检测方法,决定对克伦特罗多采集几个子集子进行定性:[img=,380,40]http://ng1.17img.cn/bbsfiles/images/2018/08/201808162301552495_1773_2166779_3.png!w380x40.jpg[/img]2ng/mL的克伦特罗标液的MRM图:[img=,690,920]http://ng1.17img.cn/bbsfiles/images/2018/08/201808162307457540_8130_2166779_3.jpg!w690x920.jpg[/img][img=,690,920]http://ng1.17img.cn/bbsfiles/images/2018/08/201808162307574590_6583_2166779_3.jpg!w690x920.jpg[/img][img=,690,920]http://ng1.17img.cn/bbsfiles/images/2018/08/201808162308050790_4421_2166779_3.jpg!w690x920.jpg[/img]通过比对标液、鸡肝样品,鸡肝样品加标的子离子碎片: 277.2>259.1、277.2>203.1、277.2>168.1的丰度比,可知鸡肝样品并未检出克伦特罗。结论:平时检测瘦肉精(克伦特罗)时,可以只采集277.2>203.1、277.2>132,但是如果遇到有检出的情况,一定要多采集几对的离子对:277.2>259.1、277.2>203.1、277.2>168.1、277.2>132进一定进行定性确认,以免出现假阳性造成误判。
有没有用到在流动相中加入三乙胺,再用盐酸调Ph的呢
国标乳品中碘的测定中,在硫酸条件下碘与丁醇反应生成丁醇与碘的衍生物,到底此衍生为何物?