本文主要研究内容
作者贾琪(2019)在《牛奶中典型化学污染物筛查方法研究》一文中研究指出:牛奶是人们日常健康饮食的重要组成部分,其安全性受到了消费者的极大关注。牛奶因直接使用或间接污染可能存在兽药、农药和霉菌毒素等多类化学污染物残留,而目前报道的技术方法多针对单一类别污染物进行检测,难以实现对多类污染物的同步快速筛查与识别。鉴于此,本论文采用液相色谱-四极杆/线性离子阱串联质谱,利用脂质组学优化前处理方法,探索前处理过程中样品基质的内在变化行为,并以此为基础研究建立了牛奶中3类209种化学污染物的风险筛查和定量确证方法,并开展了方法的评价及实际应用,具体研究结果如下:首先,利用脂质组学考察不同提取和净化条件对牛奶中不同类别脂质含量的影响。结果发现提取液中加入甲酸、乙酸或EDTA缓冲盐均会导致各类脂质产生变化,随用量的增加PC类脂质无规律性变化,PE、PS、PI三类脂质呈减少趋势,经盐析处理后,PC类脂质仍呈无规律变化,其他三类脂质与未盐析相反呈增加趋势。较高用量时盐析会引起脂质总量明显增加。不同吸附剂对脂质的吸附能力有所差异,C18对PC和PS类脂质吸附能力较强,PSA次之,而ZrO2对PE和PI类脂质的吸附能力较强。加入酸或缓冲盐对PSA和C18的吸附能力无明显影响,但加酸会引起ZrO2和EMR吸附能力下降,缓冲盐对ZrO2影响较大。不同脂质含量的提取液对化学污染物有不同的基质效应,随提取液中脂质含量的增加,各类污染物的基质效应并未表现出明显的变化规律,其中农药和霉菌毒素与兽药有所差别;当EDTA缓冲盐用量达7.5 mL时表现出基质抑制作用,而在10 mL时则表现出明显的基质增强作用,并且对各污染物的影响差异较大。其次,基于脂质组学研究和基质效应考察结果,优化了牛奶样品的QuEChERS前处理方法,筛选出2%甲酸乙腈为最优提取溶液。通过对PSA、C18、EMR、ZrO2四种吸附剂的对比考察,确定C18为最合适的吸附剂。采用UHPLC-QTRAP-MS构建化学污染物质谱信息库,综合建立了牛奶中138种兽药、55种农药和16种霉菌毒素共计209种化合物的同步筛查和定量确证方法,方法的回收率在51.20%-129.76%范围内,RSD为0.82%-19.76%,定量限在0.05?g/kg-5?g/kg之间,满足我国或欧盟规定的相关污染物的最大残留限量要求,而且在准确定量的同时可实现定性确证。最后,采用建立的筛查方法对牛奶、奶牛养殖饲料样品进行筛查分析和定性确证,发现牛奶中存在低浓度的吡虫啉、啶虫脒、磺胺二甲嘧啶、氯唑西林和黄曲霉毒素M1残留。与近年文献对比分析发现,牛奶中共有51种污染物及其代谢物有检出报道,其中80.4%为兽药。β-内酰胺类中的青霉素G和氯唑西林,喹诺酮类中的恩诺沙星和环丙沙星,磺胺类中的磺胺甲基嘧啶是相关国家中检出频率相对较高的药物,应予以优先关注。
Abstract
niu nai shi ren men ri chang jian kang yin shi de chong yao zu cheng bu fen ,ji an quan xing shou dao le xiao fei zhe de ji da guan zhu 。niu nai yin zhi jie shi yong huo jian jie wu ran ke neng cun zai shou yao 、nong yao he mei jun du su deng duo lei hua xue wu ran wu can liu ,er mu qian bao dao de ji shu fang fa duo zhen dui chan yi lei bie wu ran wu jin hang jian ce ,nan yi shi xian dui duo lei wu ran wu de tong bu kuai su shai cha yu shi bie 。jian yu ci ,ben lun wen cai yong ye xiang se pu -si ji gan /xian xing li zi jing chuan lian zhi pu ,li yong zhi zhi zu xue you hua qian chu li fang fa ,tan suo qian chu li guo cheng zhong yang pin ji zhi de nei zai bian hua hang wei ,bing yi ci wei ji chu yan jiu jian li le niu nai zhong 3lei 209chong hua xue wu ran wu de feng xian shai cha he ding liang que zheng fang fa ,bing kai zhan le fang fa de ping jia ji shi ji ying yong ,ju ti yan jiu jie guo ru xia :shou xian ,li yong zhi zhi zu xue kao cha bu tong di qu he jing hua tiao jian dui niu nai zhong bu tong lei bie zhi zhi han liang de ying xiang 。jie guo fa xian di qu ye zhong jia ru jia suan 、yi suan huo EDTAhuan chong yan jun hui dao zhi ge lei zhi zhi chan sheng bian hua ,sui yong liang de zeng jia PClei zhi zhi mo gui lv xing bian hua ,PE、PS、PIsan lei zhi zhi cheng jian shao qu shi ,jing yan xi chu li hou ,PClei zhi zhi reng cheng mo gui lv bian hua ,ji ta san lei zhi zhi yu wei yan xi xiang fan cheng zeng jia qu shi 。jiao gao yong liang shi yan xi hui yin qi zhi zhi zong liang ming xian zeng jia 。bu tong xi fu ji dui zhi zhi de xi fu neng li you suo cha yi ,C18dui PChe PSlei zhi zhi xi fu neng li jiao jiang ,PSAci zhi ,er ZrO2dui PEhe PIlei zhi zhi de xi fu neng li jiao jiang 。jia ru suan huo huan chong yan dui PSAhe C18de xi fu neng li mo ming xian ying xiang ,dan jia suan hui yin qi ZrO2he EMRxi fu neng li xia jiang ,huan chong yan dui ZrO2ying xiang jiao da 。bu tong zhi zhi han liang de di qu ye dui hua xue wu ran wu you bu tong de ji zhi xiao ying ,sui di qu ye zhong zhi zhi han liang de zeng jia ,ge lei wu ran wu de ji zhi xiao ying bing wei biao xian chu ming xian de bian hua gui lv ,ji zhong nong yao he mei jun du su yu shou yao you suo cha bie ;dang EDTAhuan chong yan yong liang da 7.5 mLshi biao xian chu ji zhi yi zhi zuo yong ,er zai 10 mLshi ze biao xian chu ming xian de ji zhi zeng jiang zuo yong ,bing ju dui ge wu ran wu de ying xiang cha yi jiao da 。ji ci ,ji yu zhi zhi zu xue yan jiu he ji zhi xiao ying kao cha jie guo ,you hua le niu nai yang pin de QuEChERSqian chu li fang fa ,shai shua chu 2%jia suan yi jing wei zui you di qu rong ye 。tong guo dui PSA、C18、EMR、ZrO2si chong xi fu ji de dui bi kao cha ,que ding C18wei zui ge kuo de xi fu ji 。cai yong UHPLC-QTRAP-MSgou jian hua xue wu ran wu zhi pu xin xi ku ,zeng ge jian li le niu nai zhong 138chong shou yao 、55chong nong yao he 16chong mei jun du su gong ji 209chong hua ge wu de tong bu shai cha he ding liang que zheng fang fa ,fang fa de hui shou lv zai 51.20%-129.76%fan wei nei ,RSDwei 0.82%-19.76%,ding liang xian zai 0.05?g/kg-5?g/kgzhi jian ,man zu wo guo huo ou meng gui ding de xiang guan wu ran wu de zui da can liu xian liang yao qiu ,er ju zai zhun que ding liang de tong shi ke shi xian ding xing que zheng 。zui hou ,cai yong jian li de shai cha fang fa dui niu nai 、nai niu yang shi si liao yang pin jin hang shai cha fen xi he ding xing que zheng ,fa xian niu nai zhong cun zai di nong du de bi chong lin 、ding chong mi 、huang an er jia mi ding 、lv zuo xi lin he huang qu mei du su M1can liu 。yu jin nian wen suo dui bi fen xi fa xian ,niu nai zhong gong you 51chong wu ran wu ji ji dai xie wu you jian chu bao dao ,ji zhong 80.4%wei shou yao 。β-nei xian an lei zhong de qing mei su Ghe lv zuo xi lin ,kui nuo tong lei zhong de en nuo sha xing he huan bing sha xing ,huang an lei zhong de huang an jia ji mi ding shi xiang guan guo jia zhong jian chu pin lv xiang dui jiao gao de yao wu ,ying yu yi you xian guan zhu 。
论文参考文献
论文详细介绍
论文作者分别是来自中国农业科学院的贾琪,发表于刊物中国农业科学院2019-07-05论文,是一篇关于牛奶论文,化学污染物论文,脂质组学论文,质谱论文,筛查论文,中国农业科学院2019-07-05论文的文章。本文可供学术参考使用,各位学者可以免费参考阅读下载,文章观点不代表本站观点,资料来自中国农业科学院2019-07-05论文网站,若本站收录的文献无意侵犯了您的著作版权,请联系我们删除。