QuEChERS/UPLC-MS/MS法快速测定土壤中吡虫啉、啶虫脒与阿维菌素残留
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摘要
[目的]建立了热带农业区水稻-辣椒轮作模式下辣椒种植季土壤中吡虫啉、啶虫脒与阿维菌残留同时快速检测方法。[方法]样品经乙腈-0.1%甲酸(V/V)提取、N-丙基乙二胺(PSA)与C_(18)混合分散剂净化,利用超高效液相色谱串联质谱(UPLC-MS/MS)与基质溶液匹配的外标法定量分析。[结果] 3种目标农药线性范围均超过3个数量级;3种添加质量分数(1.0、10.0、100.0μg/kg),土壤中3种农药平均回收率为63.7%～89.9%,相对标准偏差(RSD,n=3)为0.1%～13.6%;方法检出限(LOD,S/N=3)为0.06～0.26μg/kg,定量限(LOQ,S/N=10)为0.21～0.89μg/kg,均低于中国、欧盟辣椒中推荐最大残留限量值检测浓度。[结论]方法快速、简便、灵敏度高、重现性好,可满足实际检测需求。
[Aims] A simultaneous analysis method was optimized for the rapid determination of 3 kinds of pesticide residues in tropical soil under rice-vegetables rotation using QuEChERS-ultra-high performance liquid chromatographymass spectrometry(QuEChERS/UPLC-MS/MS). [Methods] The avermectin, imidacloprid and acetamiprid residues were effectively extracted with acetonitrile-0.1% formic acid(by vol), and then were simultaneously detected by external standard method after being purified with the mixed solid-phase dispersion of N-propylethylenedia-mine(PSA) and C_(18).[Results] The linear ranges were over 3 orders of magnitude for 3 kinds of pesticides. Under the three spiked levels of 1.0, 10.0 and 100.0 μg/kg, the average recoveries of the established method were 63.7-101.4%, with the relative standard deviation(RSD) of 0.1-13.6%(n=3). The limits of detection(LODs, S/N=3) of the established method were0.06-0.26 μg/kg, and also the limits of quantification(LOQs, S/N=10) were 0.21-0.89 μg/kg, which were all lower than concentration of the maximum residual limits for pepper recommended from China and UN. [Conclusions] The established method was rapid, easy operation, good sensitivity and reproducibility, could meet actual sample requirements for detection of pesticide residues.
[Aims] A simultaneous analysis method was optimized for the rapid determination of 3 kinds of pesticide residues in tropical soil under rice-vegetables rotation using QuEChERS-ultra-high performance liquid chromatographymass spectrometry(QuEChERS/UPLC-MS/MS). [Methods] The avermectin, imidacloprid and acetamiprid residues were effectively extracted with acetonitrile-0.1% formic acid(by vol), and then were simultaneously detected by external standard method after being purified with the mixed solid-phase dispersion of N-propylethylenedia-mine(PSA) and C_(18).[Results] The linear ranges were over 3 orders of magnitude for 3 kinds of pesticides. Under the three spiked levels of 1.0, 10.0 and 100.0 μg/kg, the average recoveries of the established method were 63.7-101.4%, with the relative standard deviation(RSD) of 0.1-13.6%(n=3). The limits of detection(LODs, S/N=3) of the established method were0.06-0.26 μg/kg, and also the limits of quantification(LOQs, S/N=10) were 0.21-0.89 μg/kg, which were all lower than concentration of the maximum residual limits for pepper recommended from China and UN. [Conclusions] The established method was rapid, easy operation, good sensitivity and reproducibility, could meet actual sample requirements for detection of pesticide residues.
引文
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[2]李启双,赖有林,张利添.稻菜轮作套种技术的优势及推广建议[J].广东农业科学,2007(4):87-89.
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[5]董同喜,杨海雪,李花粉,等.华北农田小麦-玉米轮作体系下土壤重金属积累特征研究[J].农业资源与环境学报,2014,31(4)355-365.
[6]ANDREU V,PIC魷Y.Determination of Pesticides and Their Degradation Products in Soil:Critical Review and Comparison of Methods[J].Tr AC-Trend Anal Chem,2004,23(10/11):772-789.
[7]徐宜宏,黄莹滢,裴程程,等.Qu ECh ERS-气相色谱质谱法同时测定土壤中多种常见多氯联苯及有机氯农药[J].农药,2018,57(5):351-354.
[8]成昊,张丽君,张磊,等.基质固相分散萃取-分散液相微萃取-气相色谱质谱法测定土壤中拟除虫菊酯类农药[J].分析化学,2015,43(1):137-140.
[9]ALDER L,GREULICH K,KEMPE G,et al.Residue Analysis of 500 High Priority Pesticides:Better by GC-MS or LC-MS/MS[J].Mass Spectrom Rev,2006,25(6):838-865.
[10]郭礼强,丁葵英,张金玲,等.液相色谱-串联质谱法测定土壤中19种氨基甲酸酯类农药[J].分析试验室,2016,35(2):214-219.
[11]CAI Yi-ping,SUN Zhi-wei,WANG Xiao-yan,et al.Determination of Plant Growth Regulators in Vegetable by High Performance Liquid Chromatography-tandem Mass Spectrometry Coupled with Isotop-coded Derivatization[J].Chinese J Anal Chem,2015,43(3):419-423.
[12]诸力,王晨,陈红平,等.超高效液相色谱-串联质谱法同时测定茶叶中11种植物生长调节剂及吡虫啉,啶虫脒的残留[J].分析化学,2017,45(4):529-536.
[13]梅梅,杜振霞,陈芸.Qu EChERS-超高效液相色谱串联质谱法同时测定土壤中5种常用除草剂[J].分析化学,2011,39(11):1659-1664.
[14]建峰,赵建晖,熊刚,等.超高效液相色谱-串联质谱法快速测定葱、姜、蒜与辣椒酱中的66种有机磷农药残留[J].分析测试学报,2011,30(10):1094-1099.
[15]ANASTASSIADES M,LEHOTAY S J,譒TAJNBAHER 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].JAOAC Int,2003,86(2):412-431.
[16]DRO Z觶D Z觶Y NSKI D,KOWALSK A J.Rapid Analysis of Organic Farming Insecticides in Soil and Produce Using Ultraperformance Liquid Chromatography/Tandem Mass Spectrometry[J].Anal Bioanal Chem,2009,394(8):2241-2247.
[17]孔志强,董丰收,刘新刚,等.超高效液相色谱-串联质谱法测定柑橘及柑橘精油中4种农药残留[J].分析化学,2012,40(3):474-477.
[18]赵肖华,曹赵云,牟仁祥,等.液相色谱-串联质谱法测定蔬菜、水果中5种阿维菌素类药物残留量[J].分析测试学报,2012,31(10):1266-1271.
[19]宋世明,陈兆杰,韦婕,等.Qu ECh ERS-高效液相色谱-串联质谱法测定多果定在黄瓜和土壤中的残留及消解动态[J].环境化学,2017,36(10):2165-2171.
[20]孙敏,曹赵云,刘慧,等.PSA分散固相萃取和高效液相色谱-质谱法测定蔬菜中多杀菌素的残留量[J].分析试验室,2010,29(8):70-74.
[21]刘惠君,郑巍,刘维屏.新农药吡虫啉及其代谢产物对土壤呼吸的影响[J].环境科学,2001,22(4):73-76.
[22]王彦华,陈丽萍,赵学平,等.新烟碱类和阿维菌素类药剂对蚯蚓的急性毒性效应[J].农业环境科学学报,2010,29(12):2299-2304.
[2]李启双,赖有林,张利添.稻菜轮作套种技术的优势及推广建议[J].广东农业科学,2007(4):87-89.
[3]谢妍.海南生态循环农业发展的建议[EB/OL].(2016-02-02)[2018-05-31].Http://hnrb.hinews.cn/html/2016-02/02/content_8_3.htm.
[4]张信艳.“政府-社会”互动模式下的食品安全治理研究-以“海南毒豇豆事件”为例[J].现代经济信息,2010(4):195.
[5]董同喜,杨海雪,李花粉,等.华北农田小麦-玉米轮作体系下土壤重金属积累特征研究[J].农业资源与环境学报,2014,31(4)355-365.
[6]ANDREU V,PIC魷Y.Determination of Pesticides and Their Degradation Products in Soil:Critical Review and Comparison of Methods[J].Tr AC-Trend Anal Chem,2004,23(10/11):772-789.
[7]徐宜宏,黄莹滢,裴程程,等.Qu ECh ERS-气相色谱质谱法同时测定土壤中多种常见多氯联苯及有机氯农药[J].农药,2018,57(5):351-354.
[8]成昊,张丽君,张磊,等.基质固相分散萃取-分散液相微萃取-气相色谱质谱法测定土壤中拟除虫菊酯类农药[J].分析化学,2015,43(1):137-140.
[9]ALDER L,GREULICH K,KEMPE G,et al.Residue Analysis of 500 High Priority Pesticides:Better by GC-MS or LC-MS/MS[J].Mass Spectrom Rev,2006,25(6):838-865.
[10]郭礼强,丁葵英,张金玲,等.液相色谱-串联质谱法测定土壤中19种氨基甲酸酯类农药[J].分析试验室,2016,35(2):214-219.
[11]CAI Yi-ping,SUN Zhi-wei,WANG Xiao-yan,et al.Determination of Plant Growth Regulators in Vegetable by High Performance Liquid Chromatography-tandem Mass Spectrometry Coupled with Isotop-coded Derivatization[J].Chinese J Anal Chem,2015,43(3):419-423.
[12]诸力,王晨,陈红平,等.超高效液相色谱-串联质谱法同时测定茶叶中11种植物生长调节剂及吡虫啉,啶虫脒的残留[J].分析化学,2017,45(4):529-536.
[13]梅梅,杜振霞,陈芸.Qu EChERS-超高效液相色谱串联质谱法同时测定土壤中5种常用除草剂[J].分析化学,2011,39(11):1659-1664.
[14]建峰,赵建晖,熊刚,等.超高效液相色谱-串联质谱法快速测定葱、姜、蒜与辣椒酱中的66种有机磷农药残留[J].分析测试学报,2011,30(10):1094-1099.
[15]ANASTASSIADES M,LEHOTAY S J,譒TAJNBAHER 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].JAOAC Int,2003,86(2):412-431.
[16]DRO Z觶D Z觶Y NSKI D,KOWALSK A J.Rapid Analysis of Organic Farming Insecticides in Soil and Produce Using Ultraperformance Liquid Chromatography/Tandem Mass Spectrometry[J].Anal Bioanal Chem,2009,394(8):2241-2247.
[17]孔志强,董丰收,刘新刚,等.超高效液相色谱-串联质谱法测定柑橘及柑橘精油中4种农药残留[J].分析化学,2012,40(3):474-477.
[18]赵肖华,曹赵云,牟仁祥,等.液相色谱-串联质谱法测定蔬菜、水果中5种阿维菌素类药物残留量[J].分析测试学报,2012,31(10):1266-1271.
[19]宋世明,陈兆杰,韦婕,等.Qu ECh ERS-高效液相色谱-串联质谱法测定多果定在黄瓜和土壤中的残留及消解动态[J].环境化学,2017,36(10):2165-2171.
[20]孙敏,曹赵云,刘慧,等.PSA分散固相萃取和高效液相色谱-质谱法测定蔬菜中多杀菌素的残留量[J].分析试验室,2010,29(8):70-74.
[21]刘惠君,郑巍,刘维屏.新农药吡虫啉及其代谢产物对土壤呼吸的影响[J].环境科学,2001,22(4):73-76.
[22]王彦华,陈丽萍,赵学平,等.新烟碱类和阿维菌素类药剂对蚯蚓的急性毒性效应[J].农业环境科学学报,2010,29(12):2299-2304.