摘要
目的:建立了液相色谱-串联质谱法测定猪肝中沙罗拉纳残留量的测定方法,并对方法耐用性进行了研究,旨在找出对检测结果有重大影响的因素。方法:检测方法对样品前处理、色谱条件等环节进行了考察,样品经乙腈超声提取,PRiME HLB固相萃取小柱净化,净化液氮吹近干,甲醇复溶,过膜,滤液供液相色谱-串联质谱测定;采用国际化学家协会编制的《AOAC分析方法手册》中推荐的方法,考察了测定过程中不能刻意控制的10个微小因素对检测结果准确度的影响,分别以各影响因素两个水平的差值来表示影响的大小。结果:本次测试了猪肝中沙罗拉纳的残留量,其在0~200 ng·mL^(-1)线性关系良好,y=22.09x+28.32,r^(2)=0.999;耐用性试验结果表明,检测时间的差值较大,其余影响因素的差别不明显,分别运用t检验、各因素差值与标准差比较两种统计方法对耐用性实验结果进行评价,两种方法的评价结果基本一致,对检测结果准确度影响最大的是检测时间,实际检测工作中应及时测试处理好的样品,减少因长时间放置对检测结果的影响。结论:该检测方法操作过程简单,检测速度快,选择性强,灵敏度高,可作为猪肝中沙罗拉纳残留量的检测方法;耐用性试验为检测方法开展协同试验提供了技术支撑。
A method for the determination of residue of sarolaner in porcine liver by liquid chromatographytandem mass spectrometry(LC-MS)was established,and the robustness of the method was studied,in order to find out the factors that have a significant impact on the detection results.Method:The detection method investigated the sample preparation and chromatographic conditions.The samples were extracted by acetonitrile ultrasound,PRiME HLB solid phase extraction cartridge purification,purified liquid nitrogen blowing near drying,methanol reconstitution,membrane,filtrate for LC-MS.Using the method recommended in statistical manual of the AOAC Analysis Method Manual.The influence of 10 tiny factors that could not be deliberately controlled on the accuracy of the test results was investigated.The influence was expressed by the difference of two levels of each influencing factor.Result:The residual amount of sarolane in pig liver was tested this time,and its linear relationship was good within 0~200 ng·mL^(-1),y=22.09x+28.32,r^(2)=0.999;The robustness test results show that the difference of detection time was large,and the difference of other influencing factors was not obvious.The two statistical methods of t-test and the comparison between the difference of each factor and the standard deviation are respectively used to evaluate the durability test results.The evaluation results of the two methods are basically the same.The biggest impact on the accuracy of the test results is the test time.In the actual test work,the processed samples should be tested in time to reduce the impact on the test results due to long-time storage.Conclusion:The results show that the detection method is simple in operation,fast in detection speed,strong in selectivity and high in sensitivity,and can be used as a detection method for sarolaner residue in porcine liver.
作者
夏玉吉
陈华凤
窦明理
武首薰
何楠
王毅
XIA Yuji;CHEN Huafeng;DOU Mingli;WU Shouxun;HE Nan;WANG Yi(Sichuan Institute of Food Inspection,Chengdu 610097,China;Key Laboratory of Baijiu Supervising Technology for State Market Regulation,Chengdu 610097,China;Sichuan University,Chengdu 610000,China)
出处
《食品安全导刊》
2023年第19期106-111,共6页
China Food Safety Magazine
基金
四川省市场监督管理局科技计划项目(SCSJ2021017)。
