多重吸附同步净化-气相色谱-质谱法测定干性样品中丁烯氟虫腈的残留量

引用本文: 丁立平, 郭菁, 郑铃, 陈春添, 陈志涛. 多重吸附同步净化-气相色谱-质谱法测定干性样品中丁烯氟虫腈的残留量[J]. 色谱, 2013, 31(8): 747-752. doi: 10.3724/SP.J.1123.2013.01033 shu

Citation: DING Liping, GUO Jing, ZHENG Ling, CHEN Chuntian, CHEN Zhitao. Determination of butene-fipronil residue in dry samples by multiple adsorption synchronous purification-gas chromatography-mass spectrometry[J]. Chinese Journal of Chromatography, 2013, 31(8): 747-752. doi: 10.3724/SP.J.1123.2013.01033 shu

多重吸附同步净化-气相色谱-质谱法测定干性样品中丁烯氟虫腈的残留量

通讯作者: 丁立平

基金项目:
福建出入境检验检疫局项目(FK2011-61). (FK2011-61)

摘要: 建立了干性样品中丁烯氟虫腈残留量的多重吸附同步净化(MASP)-气相色谱-质谱检测方法。前处理以1%乙酸-乙腈提取样品,应用MASP法对样品同时进行提取、盐析和净化,并利用气相色谱-质谱仪在选择离子扫描(SIM)模式下进行检测,以基质匹配标准溶液外标法定量。结果表明:丁烯氟虫腈在2~100 μg/L范围内线性关系良好,相关系数(r²)不小于0.999;在2~10 μg/kg添加水平范围内,丁烯氟虫腈的平均回收率为92.2%~97.5%,相对标准偏差(RSD, n=6)为2.69%~5.21%;方法检出限(S/N=3)为2 μg/kg;定量限(S/N=10)为6 μg/kg。本方法操作简便、快速、准确,可用于干性样品中丁烯氟虫腈的日常检测。同时,对丁烯氟虫腈的裂解机理进行了探讨。

关键词:

English

Determination of butene-fipronil residue in dry samples by multiple adsorption synchronous purification-gas chromatography-mass spectrometry

1.
Fuqing Entry-Exit Inspection and Quarantine Bureau, Fuqing 350300, China

Corresponding author: 丁立平

Received Date: 17 January 2013
Fund Project:
福建出入境检验检疫局项目(FK2011-61).

Abstract: A method was developed for the determination of butene-fipronil residue in dry samples by multiple adsorption synchronous purification (MASP)-gas chromatography (GC)-mass spectrometry (MS). After extracted with 1% acetic acid-acetonitrile, the samples were pretreated with MASP method including extraction, salting-out and purification procedures, and analyzed with GC-MS under the selected ion monitoring (SIM) mode, and then quantified by matrix-match standard solution with external standard method. The results showed good linearity in the range of 2-100 μg/L with the correlation coefficients (r²)not less than 0.999. The average fortified recovery of butene-fipronil in samples was found in the range of 92.2%-97.5% at three fortified levels from 2 to 10 μg/kg, with the relative standard deviations of 2.69%-5.21% (n=6). The limit of detection (S/N=3) for butane-fipronil was 2 μg/kg and the limit of quantification (S/N=10) was 6 μg/kg. The method is simple, rapid and accurate, and could be used for the routine analysis of butane-fipronil in dry samples. Meanwhile, the pyrolysis mechanism of butane-fipronil, as a new substance, is discussed.

Key words:

multiple adsorption synchronous purification (MASP)
/ gas chromatography-mass spectrometry (GC-MS)
/ butene-fipronil
/ residue
/ dry samples

1. [1] Dalian RUIZE Pesticide Co., Ltd. World Pesticides (大连瑞泽农药股份有限公司. 世界农药), 2005, 27(5): 49[1] Dalian RUIZE Pesticide Co., Ltd. World Pesticides (大连瑞泽农药股份有限公司. 世界农药), 2005, 27(5): 49
2. [2] Niu H T, Luo W C, Jiang G Q, et al. Acta Phytophylacica Sinica (牛洪涛, 罗万春, 江改青, 等. 植物保护学报), 2007, 34(3): 316[2] Niu H T, Luo W C, Jiang G Q, et al. Acta Phytophylacica Sinica (牛洪涛, 罗万春, 江改青, 等. 植物保护学报), 2007, 34(3): 316
3. [3] Li Q, Du J X, Zhang L. China Plant Protection (李前, 杜建雄, 张龙. 中国植保导刊), 2007(11): 39[3] Li Q, Du J X, Zhang L. China Plant Protection (李前, 杜建雄, 张龙. 中国植保导刊), 2007(11): 39
4. [4] Ding L P. Analysis and Testing Technology and Instruments (丁立平. 分析测试技术与仪器), 2010, 16(3): 191[4] Ding L P. Analysis and Testing Technology and Instruments (丁立平. 分析测试技术与仪器), 2010, 16(3): 191
5. [5] Ding L P. Analysis and Testing Technology and Instruments (丁立平. 分析测试技术与仪器), 2011, 17(3): 149[5] Ding L P. Analysis and Testing Technology and Instruments (丁立平. 分析测试技术与仪器), 2011, 17(3): 149
6. [6] Feng D Q, Ouyang G P, Kong L H. Guangzhou Chemical Industry (冯道全, 欧阳贵平, 孔令华. 广州化工), 2009, 37(3): 8[6] Feng D Q, Ouyang G P, Kong L H. Guangzhou Chemical Industry (冯道全, 欧阳贵平, 孔令华. 广州化工), 2009, 37(3): 8
7. [7] Ding H Y, Xie W, Liu H S. Journal of Instrumental Analysis (丁慧瑛, 谢文, 刘海山. 分析测试学报), 2005, 24(5): 113[7] Ding H Y, Xie W, Liu H S. Journal of Instrumental Analysis (丁慧瑛, 谢文, 刘海山. 分析测试学报), 2005, 24(5): 113
8. [8] Cao H Q, Shi Y H, Hua R M, et al. Food Science (操海群, 施艳红, 花日茂, 等. 食品科学), 2005, 26(9): 377[8] Cao H Q, Shi Y H, Hua R M, et al. Food Science (操海群, 施艳红, 花日茂, 等. 食品科学), 2005, 26(9): 377
9. [9] Guo M, Zong L G, Shan Z J, et al. Journal of Agro-Environment Science (郭敏, 宗良纲, 单正军, 等. 农业环境科学学报), 2008, 27(5): 2114[9] Guo M, Zong L G, Shan Z J, et al. Journal of Agro-Environment Science (郭敏, 宗良纲, 单正军, 等. 农业环境科学学报), 2008, 27(5): 2114
10. [10] Wu Z P, Gao W, Yan C R, et al. Modern Agrochemicals (武中平, 高巍, 颜春荣, 等. 现代农药), 2006, 5(2): 21[10] Wu Z P, Gao W, Yan C R, et al. Modern Agrochemicals (武中平, 高巍, 颜春荣, 等. 现代农药), 2006, 5(2): 21
11. [11] Zhou Y, Xu D M, Chen D J, et al. Chinese Journal of Chromatography (周昱, 徐敦明, 陈达捷, 等. 色谱), 2011, 29(7): 656[11] Zhou Y, Xu D M, Chen D J, et al. Chinese Journal of Chromatography (周昱, 徐敦明, 陈达捷, 等. 色谱), 2011, 29(7): 656
12. [12] Liu Y, Ji M S, Hu R, et al. Journal of Anhui Agriculture Science (刘郁, 纪明山, 胡睿, 等. 安徽农业科学), 2007, 35(18): 5344[12] Liu Y, Ji M S, Hu R, et al. Journal of Anhui Agriculture Science (刘郁, 纪明山, 胡睿, 等. 安徽农业科学), 2007, 35(18): 5344
13. [13] Liu Y, Yu Y H, Bian Y Q, et al. World Pesticides (刘郁, 于亚辉, 边应权, 等. 世界农药), 2008, 30(5): 35[13] Liu Y, Yu Y H, Bian Y Q, et al. World Pesticides (刘郁, 于亚辉, 边应权, 等. 世界农药), 2008, 30(5): 35
14. [14] Cao W Q, Zhao H T, She Y X, et al. Journal of Instrumental Analysis (曹维强, 赵海田, 佘永新, 等. 分析测试学报), 2009, 28(9): 1096[14] Cao W Q, Zhao H T, She Y X, et al. Journal of Instrumental Analysis (曹维强, 赵海田, 佘永新, 等. 分析测试学报), 2009, 28(9): 1096
15. [15] Anastassiades M, Lehotay S J, Stajnbaher D, et al. J AOAC Int, 2003, 86(2): 412[15] Anastassiades M, Lehotay S J, Stajnbaher D, et al. J AOAC Int, 2003, 86(2): 412
16. [16] Gong X M, Dong J, Sun J, et al. Journal of Instrumental Analysis (宫小明, 董静, 孙军, 等. 分析测试学报), 2010, 29(9): 933[16] Gong X M, Dong J, Sun J, et al. Journal of Instrumental Analysis (宫小明, 董静, 孙军, 等. 分析测试学报), 2010, 29(9): 933
17. [17] Li C Y, Kong X H, He Q, et al. Food and Nutrition in China (李春艳, 孔祥虹, 何强, 等. 中国食物与营养), 2010(2): 57[17] Li C Y, Kong X H, He Q, et al. Food and Nutrition in China (李春艳, 孔祥虹, 何强, 等. 中国食物与营养), 2010(2): 57
18. [18] Rawn D F K, Judge J, Roscoe V. Anal Bioanal Chem, 2010, 397: 2525 [18] Rawn D F K, Judge J, Roscoe V. Anal Bioanal Chem, 2010, 397: 2525
19. [19] Forsberg N D, Wilson G R, Anderson K A. J Agric Food Chem, 2011, 59(15): 8108 [19] Forsberg N D, Wilson G R, Anderson K A. J Agric Food Chem, 2011, 59(15): 8108
20. [20] Li X S, Jiang Y P, Shan W L, et al. Bull Environ Contam Toxicol, 2010, 84: 596 [20] Li X S, Jiang Y P, Shan W L, et al. Bull Environ Contam Toxicol, 2010, 84: 596
21. [21] Lucini L, Molinari G P. J Chromatogr Sci, 2011, 49: 709 [21] Lucini L, Molinari G P. J Chromatogr Sci, 2011, 49: 709
22. [22] Ding L P, Wei Y H. Agrochemicals (丁立平, 魏云昊. 农药), 2011, 50(5): 352[22] Ding L P, Wei Y H. Agrochemicals (丁立平, 魏云昊. 农药), 2011, 50(5): 352
23. [23] Xu P J, Gao X S, Tao B, et al. Chinese Journal of Analytical Chemistry (许鹏军, 高晓莎, 陶晡, 等. 分析化学), 2008, 36(11): 1515[23] Xu P J, Gao X S, Tao B, et al. Chinese Journal of Analytical Chemistry (许鹏军, 高晓莎, 陶晡, 等. 分析化学), 2008, 36(11): 1515

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

多重吸附同步净化-气相色谱-质谱法测定干性样品中丁烯氟虫腈的残留量

通讯作者: 丁立平

English

Determination of butene-fipronil residue in dry samples by multiple adsorption synchronous purification-gas chromatography-mass spectrometry

Corresponding author: 丁立平

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

多重吸附同步净化-气相色谱-质谱法测定干性样品中丁烯氟虫腈的残留量

通讯作者: 丁立平

English

Determination of butene-fipronil residue in dry samples by multiple adsorption synchronous purification-gas chromatography-mass spectrometry

Corresponding author: 丁立平

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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