高效液相色谱-串联质谱法快速检测马铃薯与土壤中氟醚菌酰胺残留

冯义志; 李颖; 金杰; 潘金菊; 唐剑峰; 齐晓雪; 梁林; 张爱娟; 刘伟

doi:10.16801/j.issn.1008-7303.2017.0106

高效液相色谱-串联质谱法快速检测马铃薯与土壤中氟醚菌酰胺残留

doi: 10.16801/j.issn.1008-7303.2017.0106

1.
山东省农药科学研究院山东省化学农药重点实验室, 济南 250033
2.
山东省联合农药工业有限公司, 济南 250100

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出版历程
- 收稿日期: 2017-08-02
- 刊出日期: 2017-12-14

Determination of LH-2010A residues in potato and soil

1.
Key Laboratory for Chemical Pesticide of Shandong Province, Shandong Academy of Pesticide Sciences, Ji'nan 250033, China
2.
Shandong United Pesticide Industry Co., Ltd., Ji'nan 250100, China

摘要

摘要: 建立了采用QuEChERS为样品前处理方法的高效液相色谱-串联质谱（HPLC-MS/MS）快速检测马铃薯和土壤中氟醚菌酰胺残留的分析方法。样品经乙腈提取，PSA、C18吸附剂净化，电喷雾电离、正离子模式采集，多反应监测模式检测，基质匹配标准品外标法定量。结果表明：在0.002~1 mg/L范围内，氟醚菌酰胺在马铃薯等基质中的质量浓度与对应的峰面积间呈良好的线性关系，其相关系数均大于0.999 9。在 0.005~0.5 mg/kg添加水平下，氟醚菌酰胺在马铃薯、马铃薯植株和土壤中的日内平均回收率为81%~98%，日内相对标准偏差（RSD）为2.2%~13%（n = 5）；日间平均回收率为75%~106%，日间RSD为0.6%~11%（n = 15）。氟醚菌酰胺在马铃薯等基质中的定量限（LOQ）（S/N=10）均为0.001mg/kg。该方法简便、快速、准确，可用于马铃薯中氟醚菌酰胺的残留检测。
- 高效液相色谱-串联质谱 /
- 马铃薯 /
- 土壤 /
- 杀菌剂 /
- 氟醚菌酰胺 /
- 残留
Abstract: A rapid and sensitive analytical method for the determination of LH-2010A residues in potato and soil was established based on QuEChERS(Quick, Easy, Cheap, Effective, Rugged and Safe) and high performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS). The samples were extracted with acetonitrile, and purified with primary secondary amine (PSA) and octadecylsilane (C18). The mass spectrometer was performed in multi-reaction monitoring mode, and electrospray ionization in positive mode was selected. The LH-2010A residues were quantified by the external standard method using the matched standard solution to compensate for matrix effect. The results indicated that the calibration curves of LH-2010A were linear in the range of 0.002-1 mg/L with correlation coefficients of more than 0.999 9. When the addition level ranged from 0.005 to 0.5mg/kg, the intra-day average recoveries of LH-2010A in potato, potato plant and soil were 81%-98%, and the relative standard deviation (RSD) ranged from 2.2% to 13% (n = 5). The inter-day average recoveries of LH-2010A were 75%-106%, and with RSD ranged from 0.6% to 11% (n = 15). The limit of quantitation (LOQ) were 0.001 mg/kg in different matrices. This method is simple, rapid and accurate, and can be adapted for the confirmation of LH-2010A residues in potato samples.
- high performance liquid chromatography-tandem mass spectrometry /
- potato /
- soil /
- fungicide /
- LH-2010A /
- residues

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参考文献(19)

张化霜, 翟明涛, 王开运, 等. 新化合物氟醚菌酰胺的抑菌活性及其对棉花立枯丝核菌的作用方式研究[J]. 农药学学报, 2013, 15(4): 405-411.

ZHANG H S, ZHAI M T, WANG K Y, et al. Study on fungicidal activity and mode of action of a novel fungicidal agent, LH-2010A against Rhoizoctonia solani [J]. Chin J Pestic Sci, 2013, 15(4): 405-411.

翟明涛, 张化霜, 王红艳, 等. 氟醚菌酰胺和5种常用杀菌剂对辣椒疫霉菌不同子实体的毒力比较[J]. 农药, 2013, 52(10): 765-767.

ZHAI M T, ZHANG H S, WANG H Y, et al. Comparison of the toxicity of LH-2010A with several conventional fungicides against Phytophthora capsici's different fruiting bodies [J]. Agrochemicals, 2013, 52(10): 765-767.

张睿, 许辉, 唐剑锋, 等. 新型杀菌剂氟醚菌酰胺对黄瓜霜霉病的毒力和田间药效评价[J]. 农药, 2013, 52(8): 596-598.

ZHANG R, XU H, TANG J F, et al. The evaluation of toxicity and field efficacy of a new fungicide LH-2010A against cucumber downy mildew [J]. Agrochemicals, 2013, 52(8): 596-598.

翟明涛. 辣椒疫霉对氟醚菌酰胺的抗性风险评价[D]. 泰安: 山东农业大学, 2014.ZHAI M T. Resistance-risk assessment of Phytophthora capsici to LH-2010A[D]. Taian: Shandong Agricultural University, 2014.

HE L, YUAN H Z, TANG J F, et al. Preliminary studies on the action mechanism of the novel fungicide LH-2010A against Phytophthora capsici [J]. Chin J Pestic Sci, 2016, 18(2): 185-193.

FAN X Q, ZHAN X P, MA L. Determination of 15 pesticide residues including fluopicolide in vegetable by dispersive solid phase cleanup and GC [J]. Mod Agrochem, 2014, 13(1): 41-43.

张秀焕. 水稻纹枯病菌对氟醚菌酰胺的抗性风险评价[D]. 泰安: 山东农业大学, 2015.ZHANG X H. The resistance risk assessment of Rhizoctonia solani to LH-2010A[D]. Taian: Shandong Agricultural University, 2015.

CHEN L, JING L G. Determination of the fluopicolide residue in the tomato fruit and the soil via UPLC-MS/MS [J]. J Saf Environ, 2017, 17(1): 341-345.

何玲, 袁会珠, 唐剑锋, 等. 新型杀菌剂氟醚菌酰胺对辣椒疫霉的作用机制初探[J]. 农药学学报, 2016, 18(2): 185-193.

樊晓青, 占绣萍, 马琳. 分散固相净化-气相色谱法检测蔬菜中氟吡菌胺等15种农药残留[J]. 现代农药, 2014, 13(1): 41-43.

MOHAPATRA S, AHUJA A K, DEEPA M, et al. Persistence and dissipation of fluopicolide in/on grape berries and soil under semi arid tropical climatic conditions of India [J]. Bull Environ Contam Toxicol, 2011, 86(2): 238-241.

SAHOO S K, MANDAL K, KUMAR R, et al. Analysis of fluopicolide and propamocarb residues on tomato and soil using QuEChERS sample preparation method in combination with GLC and GCMS [J]. Food Anal Methods, 2014, 7(5): 1032-1042.

JIANG L L, WANG H Y, XU H, et al. Transportation behaviour of fluopicolide and its control effect against Phytophthora capsici in greenhouse tomatoes after soil application [J]. Pest Manag Sci, 2015, 71(7): 1008-1014.

陈靓, 井乐刚. 基于超高效液相色谱串联质谱法的番茄果实和土壤中氟吡菌胺残留测定[J]. 安全与环境学报, 2017, 17(1): 341-345.

ANASTASSIADES M, LEHOTAY S J, ŠTAJNBAHER D, et al. Fast and easy multiresidue method employing acetonitrile extraction/partitioning and ‘dispersive solid-phase extraction’ for the determination of pesticide residues in produce [J]. J AOAC Int, 2003, 86(2): 412-431.

LIU X G, XU J, LI Y B, et al. Rapid residue analysis of four triazolopyrimidine herbicides in soil, water, and wheat by ultra-performance liquid chromatography coupled to tandem mass spectrometry [J]. Anal Bioanal Chem, 2011, 399(7): 2539-2547.

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