摘要
[目的]针对乳制品中9种国际关注而中国暂未设定残留限量的除草剂(黄草灵、环嗪酮、茚嗪氟草胺、达草灭、磺酰草吡唑、砜吡草唑、磺酰磺隆、特丁塞隆和吡喃草酮)的精准检测,建立一种快速测定方法。[方法]采用乙腈—丙酮混合试剂(体积比8:2)超声提取目标物,提取液经分散固相萃取吸附剂氟罗里硅土(Florisil)、N-丙基乙二胺(PSA)和无水MgSO_(4)净化后,建立一种高效液相色谱—串联质谱(HPLC-MS/MS)方法进行测定。[结果]9种除草剂在7 min内完全分离,在2.00~100μg/L范围内线性关系良好(r≥0.997),检出限为0.02~0.30μg/kg,加标回收率为71.6%~104.1%,相对标准偏差为0.4%~10.3%。[结论]该方法操作简便、灵敏度高、重现性好,可用于乳制品中9种除草剂残留的快速测定。
[Objective]To establish a rapid and precise determination method for 9 herbicides(asulam,hexazinone,indaziflam,norflurazon,pyrasulfotole,pyroxasulfone,sulfosulfuron,tebuthiuron,and tepraloxydim)in dairy products that are of international concern but without established maximum residue limits(MRLs)in China.[Methods]The samples are ultrasonically extracted with acetonitrile-acetone mixed reagent(v:v=8:2),and the extract is purified by the dispersed solid-phase extraction adsorbents Florisil,N-propylethylenediamine(PSA),and anhydrous MgSO_(4).A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method is established for determination.[Results]The nine herbicides are completely separated within 7 min.Their linear relationships are good within the range of 2.00~100μg/L(r≥0.997).Their detection limits are 0.02~0.30μg/kg,spiked recoveries are 71.6%~104.1%,and relative standard deviations are 0.4%~10.3%.[Conclusion]This method is simple to operate,has high sensitivity and good reproducibility,and can be used for rapid determination of residues of the 9 herbicides in dairy products.
作者
严婉盈
何敏恒
黎明明
黄诗颖
陈雯静
沈应涛
黄嘉乐
YAN Wanying;HE Minheng;LI Mingming;HUANG Shiying;CHEN Wenjing;SHEN Yingtao;HUANG Jiale(Guangzhou Inspection and Testing Certification Group Company Limited,Guangzhou,Guangdong 511447,China;South China Agricultural University,Guangzhou,Guangdong 510642,China;Guangdong Bureau of the National Food and Strategic Reserves Administration,Guangzhou,Guangdong 510050,China)
出处
《食品与机械》
北大核心
2026年第1期50-57,共8页
Food and Machinery
基金
广州市市场监督管理局科技项目(编号:2023kj47)。
