CN103926307A - 一种快速测定乳与乳制品中三聚氰胺的方法 - Google Patents
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Abstract
本发明公开了一种快速测定乳与乳制品中三聚氰胺的方法,属于食品安全领域。乳与乳制品中的三聚氰胺用乙腈提取,使用实时直接分析离子源串联质谱(DART-MS/MS)进行定性、定量分析。质谱仪器条件:电离为正离子模式,DART离子源温度300℃,栅级电压350V,质谱质量分析器电压3000V,母离子/定量离子/定性离子:127/85/68,扫描模式:二级扫描。本发明具有样品不需经色谱分离,检测方法灵敏、准确、简便、快速等特点。
Description
技术领域
本发明属于食品安全领域,具体涉及一种快速测定乳与乳制品中三聚氰胺的方法。
背景技术
三聚氰胺是典型的三嗪类化合物,白色晶体,不可燃,无味,低毒,分子式为C3H3N6。三聚氰胺是一种用途广泛的化工产品,可以作阻燃剂、减水剂、甲醛清洁剂等,最主要的是作为生产三聚氰胺甲醛树脂(MF)的原料。三聚氰胺本身低毒,但长期摄入三聚氰胺会造成生殖、泌尿系统的损害,膀胱、肾部结石,并可进一步诱发膀胱癌。
我国禁止三聚氰胺作为食品添加剂,但由于其含氮量高,且价格比蛋白质低,因此一些不法商贩将三聚氰胺非法添加到食品和饲料中以提高蛋白质含量。在“三鹿奶粉”事件后,我国加大了对婴幼儿奶粉中三聚氰胺检测的力度。2008年10月,我国卫生部、工业和信息化部、农业部、工商总局、质检总局联合发布公告,公布了乳制品及含乳食品中三聚氰胺临时管理限量值,即婴幼儿配方乳粉中三聚氰胺的限量值为1mg/kg,液态奶(包括原料乳)、奶粉、其他配方乳粉中三聚氰胺的限量值为2.5mg/kg;含乳15%以上的其他食品中三聚氰胺的限量值为2.5mg/kg。
目前,三聚氰胺常见的检测方法有:HPLC法,HPLC-MS/MS法,GC-MS法,酶联免疫法,胶体金法等等。其中HPLC法,HPLC-MS/MS法,GC-MS法精密度高,灵敏度好,但均需对样品进行复杂的前处理和色谱分离,耗时长且成本高。酶联免疫法,胶体金法操作简便,快捷,但是特异性差,精密度低,受周围环境影响较大。
直接实时分析质谱(direct analysis in real time,DART)是一种新的质谱电离技术。其原理是直接在大气压条件下,中性或惰性气体(如氮气或氦气)经放电产生激发态原子,对该激发态原子进行快速加热和电场加速,使其解析并瞬间离子化待测样品表面的标志性化合物或待测化合物后进行质谱或串联质谱检测。DART的样品无需复杂的样品处理和制备,能在几秒钟内分析存在于气体、液体、固体或材料表面的化合物,从而减少了样品损耗,可快速进行定性和半定量分析,进而实现样品的实时直接分析。
发明内容
本发明的目的是提供一种快速测定乳与乳制品中三聚氰胺的方法。
为实现上述目的,本发明采用如下技术方案:
乳与乳制品中的三聚氰胺用乙腈提取,使用实时直接分析离子源串联质谱(DART-MS/MS)进行定性、定量分析。质谱仪器条件:电离为正离子模式,DART离子源温度300℃,栅级电压350V,质谱质量分析器电压3000V,母离子/定量离子/定性离子:127/85/68,扫描模式:二级扫描。
具体实施方式
下面通过实施例的方式进一步说明本发明,但并不因此将本发明限制在所述的实施例范围之中。
精确称取1g乳或乳制品样品或三聚氰胺标准溶液0.4mL至5mL离心管中,加入3.6mL的乙腈,涡流震荡2min。吸取离心管中上清液2μL上样。用DART离子源串联质谱测定二级离子m/z85的离子强度,采用标准曲线法定量。
质谱仪器条件:电离为正离子模式,DART离子源温度300℃,栅级电压350V,质谱质量分析器电压3000V,母离子/定量离子/定性离子:127/85/68,扫描模式:二级扫描。
实验结果表明,本发明方法测定结果与国标法一致。
最后需要注意的是,公布实施方式的目的在于帮助进一步理解本发明。但是本领域的技术人员可以理解:在不脱离本发明权利要求的精神和范围内,各种替换和修改都是可能的。因此,本发明不应局限于实施例所公开的内容。本发明要求保护的范围以权利要求书界定的范围为准。
Claims (3)
1.一种快速测定乳与乳制品中三聚氰胺的方法,其特征在于:乳与乳制品中的三聚氰胺用乙腈提取,使用实时直接分析离子源串联质谱(DART-MS/MS)进行定性、定量分析。
2.权利要求1中的实时直接分析离子源串联质谱快速测定方法,其特征在于:质谱仪器条件:电离为正离子模式,DART离子源温度300℃,栅级电压350V,质谱质量分析器电压3000V,母离子/定量离子/定性离子:127/85/68,扫描模式:二级扫描。
3.权利要求2中的扫描模式,其特征在于:选用在17eV的碰撞能量下荷质比为m/z85的子离子为定量离子,在27eV的碰撞能量下荷质比为m/z68的子离子为辅助定性离子。
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Cited By (4)
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CN104237371A (zh) * | 2014-09-11 | 2014-12-24 | 上海应用技术学院 | 一种可实现质谱仪实时直接进样分析的简易装置及其应用 |
CN104597106A (zh) * | 2014-12-24 | 2015-05-06 | 江苏科技大学 | 一种基于dart-ms/ms测定家蚕中谷丙转氨酶活力的方法 |
CN105353025A (zh) * | 2015-06-19 | 2016-02-24 | 南京工业大学 | 一种快速测定食品中罗丹明b的方法 |
CN111855634A (zh) * | 2019-04-25 | 2020-10-30 | 苏州天际创新纳米技术有限公司 | 用于乳制品中三聚氰胺检测的检测方法以及试剂盒 |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104237371A (zh) * | 2014-09-11 | 2014-12-24 | 上海应用技术学院 | 一种可实现质谱仪实时直接进样分析的简易装置及其应用 |
CN104237371B (zh) * | 2014-09-11 | 2017-01-11 | 上海应用技术学院 | 一种可实现质谱仪实时直接进样分析的简易装置及其应用 |
CN104597106A (zh) * | 2014-12-24 | 2015-05-06 | 江苏科技大学 | 一种基于dart-ms/ms测定家蚕中谷丙转氨酶活力的方法 |
CN104597106B (zh) * | 2014-12-24 | 2017-06-23 | 江苏科技大学 | 一种基于dart‑ms/ms测定家蚕中谷丙转氨酶活力的方法 |
CN105353025A (zh) * | 2015-06-19 | 2016-02-24 | 南京工业大学 | 一种快速测定食品中罗丹明b的方法 |
CN111855634A (zh) * | 2019-04-25 | 2020-10-30 | 苏州天际创新纳米技术有限公司 | 用于乳制品中三聚氰胺检测的检测方法以及试剂盒 |
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