登录    |    注册

您好,欢迎来到中国测试科技资讯平台!

首页>《中国测试》期刊>本期导读>微波萃取-气相色谱/串联质谱测定贝中有机磷农药

微波萃取-气相色谱/串联质谱测定贝中有机磷农药

1040    2018-04-30

¥0.50

全文售价

作者:于洪1, 许秀艳2, 许人骥2, 陈烨2

作者单位:1. 乌鲁木齐市环境监测中心站, 新疆 乌鲁木齐 830000;
2. 中国环境监测总站, 北京 100012


关键词:微波萃取;气相色谱/三重四级质谱联用;贝类;有机磷农残


摘要:

建立微波萃取-气相色谱/三重四级质谱法同时测定贝类中8种有机磷农药残留的方法。优化仪器分析条件,研究微波萃取溶剂、萃取温度、保持时间对萃取效果的影响。方法的线性关系良好,目标组分的检出限在0.1~0.2 g/g之间。贝类样品加标的回收率在41.2%~105%之间,相对标准偏差在3.3%~19%之间。该方法综合微波萃取快速高效以及气相色谱/三重四级质谱抗干扰强的优势,可用于贝类样品中有机磷农药残留的痕量分析。


Determination of organophosphorus pesticides in shellfish by gas chromatography-triple quadrupole mass spectrometry with microwave extraction

YU Hong1, XU Xiuyan2, XU Renji2, CHEN Ye2

1. Urumqi Environmental Monitoring Centre, Urumqi 830000, China;
2. China National Environmental Monitoring Centre, Beijing 100012, China

Abstract: A gas chromatography-triple quadrupole mass spectrometry(GC/QQQ) method coupled with microwave extraction(ME) was developed for determination of organophosphorus pesticides(OPPs) in shellfish. Instrumental parameters of GC/QQQ were optimized. Affecting factors of ME such as extraction solvent, temperature and holding time were also studied. Linear relationships of the method were good and method detection limits of targets were within range of 0.1-0.2 μg/g. Recoveries of spiked samples were 41.2%-105% and relative standard deviations were 3.3%-19%. Combined advantages of rapidity & efficiency of ME and anti-interference of GC/QQQ, the proposed method could be used for trace analysis of OPPs in shellfish.

Keywords: microwave extraction;gas chromatography/triple quadrupole mass spectrometry;shellfish;organophosphorus pesticides residue

2018, 44(4): 64-68  收稿日期: 2017-12-08;收到修改稿日期: 2018-01-12

基金项目: 水体污染控制与治理科技重大专项(2013ZX00702001)

作者简介: 于洪(1986-),男,四川泸州市人,工程师,主要从事环境有机污染物分析。

参考文献

[1] 朱岩,曹莹,张亚辉,等. 有机磷农药对锯齿新米虾的毒性及敏感性分析[J]. 中国环境科学,2017,37(2):745-753.
[2] 于志勇,金芬,孙景芳,等. 北京市场常见淡水食用鱼体内农药残留水平调查及健康风险评价[J]. 环境科学,2013, 34(1):251-256.
[3] 王薇,李清波,王晨祥,等. 辽东半岛海域鱼贝种有机氯农药残留及其风险评估[J]. 生态毒理学报,2015,10(3):135-143.
[4] 孙芳,黄云,刘志刚,等. 鄱阳湖康山和湖口水域鱼、贝类体内有机氯农药残留现状[J]. 环境科学研究,2010,23(4):467-472.
[5] 张小辉,贾海燕,祁士华,等. 汉江水体和鱼体内有机氯农药残留水平及积累特征分析[J]. 安全与环境工程,2014, 21(2):40-45.
[6] 郑远利,马莉莉,吴晓波,等. 固相萃取-高效液相色谱法测定水中3种有机磷农药残留[J]. 理化检验(化学分册),2017,53(3):355-358.
[7] 周蓉,曹赵云,赵肖华,等. 分散固相萃取-分散液液微萃取/气相色谱-串联质谱法测定蔬菜中19种有机磷农药残留[J]. 分析测试学报,2017,36(1):67-72.
[8] 张本山,于淑娟,曾新安,等. 微波萃取气相色谱法测定淀粉中14种有机氯农药残留[J]. 分析测试学报,2011,30(3):344-348.
[9] WU L J, SONG Y, HU M Z, et al. Integrated micro-wave processing system for the extraction of organopho-sphorus pesticides in fresh vegetables[J]. Talanta,2015(134):366-372.
[10] FUENTES E, BAEZ M, DIAZ J. Microwave-assisted extraction at atmospheric pressure coupled to different clean-up methods for the determination of organophosphorus pesticides in olive and avocado oil[J]. Journal of Chromatography A,2009,1216(51):8859-8866.
[11] 郭萌萌,国佼,吴海燕,等. 通过式固相萃取-液相色谱-四极杆/静电场轨道阱高分辨质谱快速筛查鱼肉中全氟化合物及其前体物质[J]. 分析化学,2016,44(10):1504-1513.
[12] KILJANEK T, NIEWIADOWSKA A, SEMENIUK S. Determination of organophosphorus pesticide residues in the live by gas chromatography with flame photometricdetection[J]. Bulletin of Veterinary Institute in Pulawy,2011,55(4):731-736.
[13] 刘庆斌,张睿,王海涛,等. 高效液相色谱串联质谱法对栀子中11种有机磷农药残留的检测[J]. 分析测试学报,2010,19(1):73-76.
[14] 庞国芳. 农药兽药残留现代分析技术[M]. 北京:科学出版社,2007:96-101.
[15] 唐玉佳,钱枫,边森. 微波萃取-紫外分光光度法测定土壤中PCBs的研究[J]. 环境科学与技术,2010,22(12):502-505.
[16] LOPEZ A V, YOUNG R, BECKERT W F. Stability of organic-pollutants during microwave-assisted extraction from solid matrics[J]. Journal of AOAC International,1998, 81(2):426-476.
[17] 郭萌萌,李兆新,王智,等. 通过式固相萃取净化/液相色谱-串联质谱法快速检测水产品中11种青霉素残留[J]. 分析测试学报,2017,36(3):337-342.