蒜苔中咪鲜胺及其代谢物残留检测方法的研究与比较

引用本文: 陈克云, 李玲, 鞠香, 王艳丽, 刘艳明. 蒜苔中咪鲜胺及其代谢物残留检测方法的研究与比较[J]. 色谱, 2020, 38(2): 232-237. doi: 10.3724/SP.J.1123.2019.04008 shu

Citation: CHEN Keyun, LI Ling, JU Xiang, WANG Yanli, LIU Yanming. Study and comparison of detection methods for prochloraz and its metabolite residue in garlic bolting[J]. Chinese Journal of Chromatography, 2020, 38(2): 232-237. doi: 10.3724/SP.J.1123.2019.04008 shu

蒜苔中咪鲜胺及其代谢物残留检测方法的研究与比较

山东省食品药品检验研究院, 山东济南 250101

通讯作者: 刘艳明, E-mail:msymliu@163.com

基金项目:
国家重点研发计划项目（2017YFC1601600）.

摘要: 建立了水解法与QuEChERS法测定蒜苔中咪鲜胺及其代谢物的残留量，并对两种方法进行了比较。在QuEChERS法中，样品经乙腈提取，QuEChERS净化管净化后用气相色谱法测定咪鲜胺及其代谢产物2，4，6-三氯苯酚的含量，基质匹配标准曲线外标法定量；在水解法中，样品经乙腈提取，吡啶盐酸盐水解后，用硫酸磺化，用气相色谱法测定咪鲜胺的含量。结果表明，水解法和QuEChERS法测定的咪鲜胺标准曲线在0.01~2 mg/L范围内均有良好的线性关系，相关系数（r²）均大于0.999。水解法中咪鲜胺的定量限（LOQ）为0.005 mg/kg；QuEChERS法中咪鲜胺的LOQ为0.039 mg/kg、2，4，6-三氯苯酚的LOQ为0.003 mg/kg。在3个不同浓度添加水平下，方法回收率为81.5%~105.4%，相对标准偏差（RSD）为1.3%~6.8%。在测定阳性样品时，水解法可以较为全面地检测出样品中咪鲜胺及其主要代谢物的总量，QuEChERS法可以检测出咪鲜胺及其主要代谢物2，4，6-三氯苯酚的存在形式和各自的含量，两种方法可以互相补充用于蒜苔中咪鲜胺及其代谢物的检测和确证。

关键词:

English

Study and comparison of detection methods for prochloraz and its metabolite residue in garlic bolting

Shandong Institute for Food and Drug Control, Jinan 250101, China

Corresponding author: LIU Yanming, msymliu@163.com

Received Date: 02 April 2019
Fund Project:
National Key Research and Development Program of China (No. 2017YFC1601600).

Abstract: Two analytical methods for the determination of prochloraz and its metabolite residues in garlic bolting were established and compared. In the QuEChERS method, the sample was extracted with acetonitrile and purified in a QuEChERS purification tube, and then, the contents of prochloraz and its metabolite 2,4,6-trichlorophenol were determined by gas chromatography. The hydrolysis method involved extraction of the sample with acetonitrile, hydrolysis by pyridine hydrochloride, purification with sulfuric acid, and determination of the prochloraz content by gas chromatography. The standard curve in the hydrolysis and QuEChERS methods showed a good linear relationship in the concentration range of 0.01-2 mg/L, and the correlation coefficient (r²) was greater than 0.999. The limit of quantitation (LOQ) for prochloraz in the hydrolysis method was 0.005 mg/kg. The LOQ for prochloraz in the QuEChERS method was 0.039 mg/kg, and that for 2,4,6-trichlorophenol was 0.003 mg/kg. At three spiked levels in the sample, the recoveries were 81.5%-105.4%, and the relative standard deviations (RSDs) were between 1.3%-6.8%. In the determination of positive samples, the hydrolysis method can detect the total amount of prochloraz and its main metabolites. QuEChERS method can detect the presence and contents of prochloraz and its main metabolite 2,4,6-trichlorophenol. These two methods can complement each other for the detection and confirmation of prochloraz and its metabolites in garlic bolting.

Key words:

1. [1] Dang K T H, Singh Z, Swinny E E. J Agric Food Chem, 2008, 56(22):10667
2. [2] Menezes F A, dos Santos F N, Pereira P A. Talanta, 2010, 81(1):346
3. [3] Kastanias M A, Chrysayi-Tokousbalides M, Coward S, et al. B Environ Contam Tox, 2006, 77(1):149
4. [4] Cengiz M F, Catal M, Erler F, et al. Anal Methods, 2014, 6(6):1970
5. [5] GB 2763-2016
6. [6] Nielsen F K, Hansen C H, Fey J A, et al. Int J Toxicol, 2015, 34(6):1
7. [7] Hass U, Christiansen S L, Poulsen L M, et al. Int J Androl, 2010, 29(1):186
8. [8] Navickiene S, Ribeiro M L. J Braz Chem Soc, 2005, 16(2):157
9. [9] Gong D X.[PhD Dissertation]. Hangzhou:Zhejiang University, 2005 龚道新.[博士学位论文]. 杭州:浙江大学, 2005
10. [10] Hameed B H. Colloid Surfaces A, 2007, 307(1):45
11. [11] Li H, Li J, Hou C, et al. Talanta, 2010, 83(2):591
12. [12] Hameed B H, Tan I A W, Ahmad A L. Chem Eng J, 2008, 144(2):235
13. [13] Jia Q L, Wang M Q. China Brewing, 2015, 34(9):145 贾巧莉, 王明强. 中国酿造, 2015, 34(9):145
14. [14] De P M, Taccheo B M, Damiano V, et al. J Chromatogr A, 1997, 765:127
15. [15] Fan X, Zhao S, Chen X, et al. Food Anal Method, 2018, 11(5):1
16. [16] Lu J W, Li R, Yang F, et al. Food Science, 2015, 36(12):213 卢俊文, 李蓉, 杨芳, 等. 食品科学, 2015, 36(12):213
17. [17] Fuse J I, Kanamori H, Ideyoshi N. J Food Hyg Soc Jpn, 2000, 41(1):61
18. [18] Polese L, Jardim E F G, Navickiene S, et al. Eclética Quím, 2006, 31(2):59

扫一扫看文章

计量

PDF下载量: 13
文章访问数: 1093
HTML全文浏览量: 198

通讯作者: 陈斌, bchen63@163.com

1.
沈阳化工大学材料科学与工程学院沈阳 110142

蒜苔中咪鲜胺及其代谢物残留检测方法的研究与比较

通讯作者: 刘艳明, E-mail:msymliu@163.com

English

Study and comparison of detection methods for prochloraz and its metabolite residue in garlic bolting

Corresponding author: LIU Yanming, msymliu@163.com

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？

计量

通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

蒜苔中咪鲜胺及其代谢物残留检测方法的研究与比较

通讯作者: 刘艳明, E-mail:msymliu@163.com

English

Study and comparison of detection methods for prochloraz and its metabolite residue in garlic bolting

Corresponding author: LIU Yanming, msymliu@163.com

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？

计量

文章相关

通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

CCS Chemistry：颜徐州、鲍哲南：你的皮肤可能是一片SPMs