QuEChERS-超高效液相色谱串联质谱法测定甜菜中15种除草剂
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摘要
[目的]建立了甜菜中15种除草剂残留量的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法。[方法]甜菜样品用乙腈提取,经QuEChERS方法净化后,在超高效液相色谱-串联质谱仪电喷雾正负离子在线切换多反应监测(MRM)模式下测定,外标法定量。[结果]15种除草剂在0.1～5.0μg/L范围内呈良好的线性关系,相关系数均大于0.996,检出限(LOD)为0.001～0.038μg/kg,定量限(LOQ)为0.004～0.127μg/kg。1.0、5.0、10.0μg/kg 3个添加水平下15种除草剂回收率范围为82.8%～109.2%,相对标准偏差为0.81%～6.4%。[结论]该方法高效、准确,灵敏度和精密度均满足甜菜多除草剂残留检测的要求。
[Aims] A method for the determination of 15 herbicide in sugarbeet by ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS) was developed. [Methods] The residues in the samples were extracted with acetonitrile, cleaned up by developed QuEChERS method. Then qualitation of the analytes was achieved with multiple reaction monitoring(MRM) and the external standard method was used for quantification.[Results] The linearity of 15 herbicides was good in the concentration ranges of 0.1 to 5.0 μg/L with correlation efficient(r2) larger than 0.996. The limits of detection(LOD) were 0.001-0.038 μg/kg and the limits of quantification(LOQ)were 0.004-0.127 μg/kg. The recoveries at three spiked levels of 1.0, 5.0 and 10.0 μg/kg ranged from 82.8 to 109.2%with the relative standard deviations(RSD)(n=6) from 0.81 to 6.4%. [Conclusions] The proposed method is rapid, exactly and characterized with acceptable sensitivity and accuracy to meet the requirements of herbicides analysis in sugarbeet.
[Aims] A method for the determination of 15 herbicide in sugarbeet by ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS) was developed. [Methods] The residues in the samples were extracted with acetonitrile, cleaned up by developed QuEChERS method. Then qualitation of the analytes was achieved with multiple reaction monitoring(MRM) and the external standard method was used for quantification.[Results] The linearity of 15 herbicides was good in the concentration ranges of 0.1 to 5.0 μg/L with correlation efficient(r2) larger than 0.996. The limits of detection(LOD) were 0.001-0.038 μg/kg and the limits of quantification(LOQ)were 0.004-0.127 μg/kg. The recoveries at three spiked levels of 1.0, 5.0 and 10.0 μg/kg ranged from 82.8 to 109.2%with the relative standard deviations(RSD)(n=6) from 0.81 to 6.4%. [Conclusions] The proposed method is rapid, exactly and characterized with acceptable sensitivity and accuracy to meet the requirements of herbicides analysis in sugarbeet.
引文
[1]李蔚农,姜莉,董戈.我国甜菜生产中除草剂应用现状及发展前景[J].中国糖料,2014(4):83-85.
[2]杜利君,花锦,赵悠悠,等.分散固相萃取-离子色谱质谱法测定水果和蔬菜中的草甘膦残留量[J].分试验室,2017,36(11):1277-1280.
[3]项盛,宗伏霖,吴学民,等.苯氧乙酸类除草剂飘移及风险评价[J].农药,2015,54(10):709-714.
[4]金晶,顾海东,高仕谦,等.超声提取-磁性固相萃取-UHPLC-MS/MS测定土壤中4种苯脲类除草剂[J].分析试验室,2017,36(1):87-91.
[5]CHOU T Y,LIN S L,FUH M R.Determination of Phenylurea Herbicides in Aqueous Samples Using Partitioned Dispersive Liquid Liquid Microextraction[J].2009,80(2):493-498.
[6]XU Chao,TU Wen-qing,DENG Mi,et al.Stereoselective Induction of Developmental Toxicity and Immunotoxicity by Acetochlor in the Early Life Ttage of Zebrafish[J].Chemosphere,2016,164:618-626.
[7]李建勋,孙梦园,胡雪艳,等.顶空固相微萃取结合气相色谱-三重四极杆质谱法快速测定茶叶中11种酰胺类除草剂残留[J].分析测试学报,2017,36(11):1339-1345.
[8]常海霞,郭红亮.除草剂对农作物影响的分析[J].山西农经,2018(5):70-71.
[9]李蔚农,姜莉,董戈.我国甜菜生产中除草剂应用现状及发展前景[J].中国糖料,2014(4):83-85.
[10]孙慧青,李义强,徐光军,等.GPC-GC同时测定烟草中10种除草剂的残留[J].农药,2014,53(3):197-199.
[11]黄敏兴,高裕锋,甄振鹏,等.气相色谱-质谱法测定甘蔗中13种除草剂[J].化学试剂,2018,40(8):759-762.
[12]杨益林,潘艳坤,周玉薇,等.液相色谱-串联质谱法测定甘蔗中10种除草剂的残留量[J].理化检验-化学分册,2017,53(5):507-509.
[13]王皙玮,刘质静,胡晓航,等.甜菜中4种除草剂残留的超高效液相色谱-串联质谱检测方法研究[J].黑龙江大学工程学报,2013,4(3):35-38.
[14]周芹,吴玉梅,许庆轩.超高效液相色谱-串联质谱法测定甜菜中除草剂残留含量[J].中国农学通报,2017,33(36):152-156.
[15]ANASTASSIADES M,LEHOTAY S J,STAJNBAHER D,et al.Fast Easy Multiresidue Method Employing Acetonitrile Extraction/Partitioning,“Dispersive Solid-phase Extraction”for the Determination of Pesticide Residues in Produce[J].Journal of AOACInternational,2003,86(2):412.
[2]杜利君,花锦,赵悠悠,等.分散固相萃取-离子色谱质谱法测定水果和蔬菜中的草甘膦残留量[J].分试验室,2017,36(11):1277-1280.
[3]项盛,宗伏霖,吴学民,等.苯氧乙酸类除草剂飘移及风险评价[J].农药,2015,54(10):709-714.
[4]金晶,顾海东,高仕谦,等.超声提取-磁性固相萃取-UHPLC-MS/MS测定土壤中4种苯脲类除草剂[J].分析试验室,2017,36(1):87-91.
[5]CHOU T Y,LIN S L,FUH M R.Determination of Phenylurea Herbicides in Aqueous Samples Using Partitioned Dispersive Liquid Liquid Microextraction[J].2009,80(2):493-498.
[6]XU Chao,TU Wen-qing,DENG Mi,et al.Stereoselective Induction of Developmental Toxicity and Immunotoxicity by Acetochlor in the Early Life Ttage of Zebrafish[J].Chemosphere,2016,164:618-626.
[7]李建勋,孙梦园,胡雪艳,等.顶空固相微萃取结合气相色谱-三重四极杆质谱法快速测定茶叶中11种酰胺类除草剂残留[J].分析测试学报,2017,36(11):1339-1345.
[8]常海霞,郭红亮.除草剂对农作物影响的分析[J].山西农经,2018(5):70-71.
[9]李蔚农,姜莉,董戈.我国甜菜生产中除草剂应用现状及发展前景[J].中国糖料,2014(4):83-85.
[10]孙慧青,李义强,徐光军,等.GPC-GC同时测定烟草中10种除草剂的残留[J].农药,2014,53(3):197-199.
[11]黄敏兴,高裕锋,甄振鹏,等.气相色谱-质谱法测定甘蔗中13种除草剂[J].化学试剂,2018,40(8):759-762.
[12]杨益林,潘艳坤,周玉薇,等.液相色谱-串联质谱法测定甘蔗中10种除草剂的残留量[J].理化检验-化学分册,2017,53(5):507-509.
[13]王皙玮,刘质静,胡晓航,等.甜菜中4种除草剂残留的超高效液相色谱-串联质谱检测方法研究[J].黑龙江大学工程学报,2013,4(3):35-38.
[14]周芹,吴玉梅,许庆轩.超高效液相色谱-串联质谱法测定甜菜中除草剂残留含量[J].中国农学通报,2017,33(36):152-156.
[15]ANASTASSIADES M,LEHOTAY S J,STAJNBAHER D,et al.Fast Easy Multiresidue Method Employing Acetonitrile Extraction/Partitioning,“Dispersive Solid-phase Extraction”for the Determination of Pesticide Residues in Produce[J].Journal of AOACInternational,2003,86(2):412.