高效液相色谱-串联质谱法快速测定果蔬中特丁硫磷、特丁硫磷砜和特丁硫磷亚砜的残留量
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摘要
目的建立高效液相色谱-串联质谱法快速测定蔬菜、水果中特丁硫磷、特丁硫磷砜和特丁硫磷亚砜农药残留量的分析方法。方法样品经乙腈直接匀浆提取过滤,滤液中加入氯化钠分层后吸取上层清液过0.22μm滤膜,经Phenomenex C_(18)(150 mm×2.0 mm, 5μm)色谱柱,以0.1%乙酸铵甲醇溶液和0.1%甲酸乙酸铵水溶液为流动相,梯度洗脱,流速为0.5mL/min,柱温为35℃,多重态反应监测模式监测。结果在14.4～288μg/L的浓度范围内,各组分线性关系良好(r>0.999),检出限为0.12～0.63μg/kg,加标回收率为84.8%～103.0%,相对标准偏差为0.473%～15.622%。结论该方法分析速度快、灵敏度高,适合于蔬菜、水果中特丁硫磷类残留物的检测。
Objective To establish a method for rapid determination of terbufos, terbufos-sulfone and terbufos-sulfoxide residues in vegetables and fruits by high performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted and filtered with acetonitrile homogenate, sodium chloride was added to the filtrate and the filtrate was filtered by0.22 microns filter membrane after the supernatant was absorbed. The samples were separated with a Phenomenex C_(18)(150 mm×2.0 mm, 5 μm)colum using 0.1% ammonium acetate in methanol and 0.1% ammonium formate acetate as mobile phase at the flow of 0.5 mL/min by gradient elute, and the column temperature was maintained at 35 ℃.The detection was monitored by multiple reaction monitoring. Results At the concentration range of 14.4-288 μg/L, the linear relationship of the components was good(r>0.999), the limits of detection were 0.12-0.63 μg/kg, the standard recoveries were 84.8%-103.0%, and the relative standard deviations were 0.473%-15.622%. Conclusion This method has the advantages of high speed analysis and high sensitivity, and is suitable for detecting terbutazone residues in vegetables and fruits.
Objective To establish a method for rapid determination of terbufos, terbufos-sulfone and terbufos-sulfoxide residues in vegetables and fruits by high performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted and filtered with acetonitrile homogenate, sodium chloride was added to the filtrate and the filtrate was filtered by0.22 microns filter membrane after the supernatant was absorbed. The samples were separated with a Phenomenex C_(18)(150 mm×2.0 mm, 5 μm)colum using 0.1% ammonium acetate in methanol and 0.1% ammonium formate acetate as mobile phase at the flow of 0.5 mL/min by gradient elute, and the column temperature was maintained at 35 ℃.The detection was monitored by multiple reaction monitoring. Results At the concentration range of 14.4-288 μg/L, the linear relationship of the components was good(r>0.999), the limits of detection were 0.12-0.63 μg/kg, the standard recoveries were 84.8%-103.0%, and the relative standard deviations were 0.473%-15.622%. Conclusion This method has the advantages of high speed analysis and high sensitivity, and is suitable for detecting terbutazone residues in vegetables and fruits.
引文
[1]中华人民共和国农业部公告第199号.公布国家明令禁止使用的农药和不得在蔬菜、果树、茶叶、中草药材上使用的高毒农药品种清单[EB/OL].[2002-6-5].http://jiuban.moa.gov.cn/zwllm/tzgg/gg/200210/t20021016_14307.htm Notice of the ministry of agriculture of the People's Republic of China No.199.To publish a list of pesticides expressly prohibited by the state and varieties of highly toxic pesticides prohibited from being used on vegetables,fruit trees,tea leaves and medicinal herbs[EB/OL].[2002-6-5].http://jiuban.moa.gov.cn/zwllm/tzgg/gg/200210/t20021016_14307.htm
[2]中华人民共和国农业部公告第1586号[EB/OL].[2011-7-5].http://jiuban.moa.gov.cn/zwllm/tzgg/gg/201107/t20110705_2045813.htm Notice of the ministry of agriculture of the People's Republic of China No.1586[EB/OL].[2011-7-5].http://jiuban.moa.gov.cn/zwllm/tzgg/gg/201107/t20110705_2045813.htm
[3]Bowman BT,Sans WW.Adsorption,desorption,soil mobility,aqueous persistence and octanol-water partitioning co-efficients of terbufos,terbufos sulfoxide,terbufos sulfone[J].Environ Sci Health B,1982,(17):447-462.
[4]GB 2763-2014食品中农药最大残留限量[S].GB 2763-2014 Maximum residue limit of pesticide in food[S].
[5]NY/T 761-2008蔬菜和水果中有机磷、有机氯、拟除虫菊酯和氨基甲酸酯类农药多残留的测定[S].NY/T 761-2008 Determination of organophosphorus,organochlorine,pyrethroid and carbamate residues in vegetables and fruits[S].
[6]NY/T 1379-2007蔬菜中334种农药多残留的测定气相色谱质谱法和液相色谱质谱法[S].NY/T 1379-2007 Determination of 334 pesticide residues in vegetables by gas chromatography-mass spectrometry and liquid chromatography-mass spectrometry[S].
[7]贺红周,范小伟,赵敬坤,等.农药样品中添加甲拌磷、特丁硫磷、对硫磷的气相色谱分析[J].南方农业,2011,5(5):53-55.He HZ,Fan XW,Zhao JK,et al.Gas chromatographic analysis of methimate,tetrathiophos and parathion was carried out in pesticide samples[J].South China Agric,2011,5(5):53-55.
[8]吴文涛,单正军.特丁硫磷在环境中的迁移性研究[J].农药学学报,2011,13(2):174-179.Wu WT,Shan ZJ.Study on the environmental mobility of tetrathiophos[J].Chin J Pestic Sci,2011,13(2):174-179.
[9]高艺羡,陈萍虹,聂丹丹.气相色谱-串联质谱双内标法测定茶叶中53种农药残留[J].色谱,2018,36(6):531-540.Gao YX,Chen PH,Nie DD.Determination of 53 pesticide residues in tea by gas chromatography-tandem mass spectrometry[J].Chin J Chromatogr,2018,36(6):531-540.
[10]张秋园,林晓旭,廖洁莹,等.气相色谱法测定蔬菜、水果中特丁硫磷砜和特丁硫磷亚砜残留量[J].山东化工,2016,45(14):57-58.Zhang QY,Lin XX,Liao JY,et al.Determination of terbutenol sulfone and tert-butyl sulfoxide residues in vegetables and fruits by gas chromatography[J].Shandong Chem Ind,2016,45(14):57-58.
[11]马杰,李青,白梅,等.QuEChERS前处理技术与在线凝胶渗透色谱-气相色谱质谱联用法测定蔬菜水果中20种农药残留[J].食品安全质量检测学报,2016,7(1):20-26.Ma J,Li Q,Bai M,et al.Determination of 20 pesticide residues in vegetables and fruits by QuEChERS pretreatment and on-line gel permeation chromatography-gas chromatography-mass spectrometry[J].JFood Saf Qual,2016,7(1):20-26.
[12]田海,谭辉华,李雪生,等.分散液相微萃取-气相色谱法快速测定甘蔗中特丁硫磷残留[J].现代农药,2012,11(2):43-46.Tian H,Tan HH,Li XS,et al.Rapid determination of tetrathiophos residues in sugarcane by dispersive liquid phase microextraction-gas chromatography[J].Mod Agrochem,2012,11(2):43-46.
[13]李俊,蔡涛,周雪丽,等.气相色谱-三重四级杆质谱法同时测定农药中32种隐性添加成分[J].食品安全质量检测学报,2018,7(9):3219-3225.Li J,Cai T,Zhou XL,et al.Simultaneous determination of 32 implicit additives in pesticides by gas chromatography-triple quadrupole mass spectrometry[J].J Food Saf Qual,2018,7(9):3219-3225.
[14]陈丽娥,董晓尉.气相色谱检测果蔬中有机磷农药残留方法[J].南方农业,2017,11(2):86-88.Chen LE,Dong XL.Determination of organophosphorus pesticide residues in fruits and vegetables by gas chromatography[J].South China Agric,2017,11(2):86-88.
[15]Catherine B,Choung,Ross V,et al.Toxicity of the insecticide terbufos,its oxidation metabolites,and the herbicide atrazine in binary mixtures to ceriodaphnia cf dubia[J].Arch Environ Contam Toxicol,2011,(60):417-425.
[2]中华人民共和国农业部公告第1586号[EB/OL].[2011-7-5].http://jiuban.moa.gov.cn/zwllm/tzgg/gg/201107/t20110705_2045813.htm Notice of the ministry of agriculture of the People's Republic of China No.1586[EB/OL].[2011-7-5].http://jiuban.moa.gov.cn/zwllm/tzgg/gg/201107/t20110705_2045813.htm
[3]Bowman BT,Sans WW.Adsorption,desorption,soil mobility,aqueous persistence and octanol-water partitioning co-efficients of terbufos,terbufos sulfoxide,terbufos sulfone[J].Environ Sci Health B,1982,(17):447-462.
[4]GB 2763-2014食品中农药最大残留限量[S].GB 2763-2014 Maximum residue limit of pesticide in food[S].
[5]NY/T 761-2008蔬菜和水果中有机磷、有机氯、拟除虫菊酯和氨基甲酸酯类农药多残留的测定[S].NY/T 761-2008 Determination of organophosphorus,organochlorine,pyrethroid and carbamate residues in vegetables and fruits[S].
[6]NY/T 1379-2007蔬菜中334种农药多残留的测定气相色谱质谱法和液相色谱质谱法[S].NY/T 1379-2007 Determination of 334 pesticide residues in vegetables by gas chromatography-mass spectrometry and liquid chromatography-mass spectrometry[S].
[7]贺红周,范小伟,赵敬坤,等.农药样品中添加甲拌磷、特丁硫磷、对硫磷的气相色谱分析[J].南方农业,2011,5(5):53-55.He HZ,Fan XW,Zhao JK,et al.Gas chromatographic analysis of methimate,tetrathiophos and parathion was carried out in pesticide samples[J].South China Agric,2011,5(5):53-55.
[8]吴文涛,单正军.特丁硫磷在环境中的迁移性研究[J].农药学学报,2011,13(2):174-179.Wu WT,Shan ZJ.Study on the environmental mobility of tetrathiophos[J].Chin J Pestic Sci,2011,13(2):174-179.
[9]高艺羡,陈萍虹,聂丹丹.气相色谱-串联质谱双内标法测定茶叶中53种农药残留[J].色谱,2018,36(6):531-540.Gao YX,Chen PH,Nie DD.Determination of 53 pesticide residues in tea by gas chromatography-tandem mass spectrometry[J].Chin J Chromatogr,2018,36(6):531-540.
[10]张秋园,林晓旭,廖洁莹,等.气相色谱法测定蔬菜、水果中特丁硫磷砜和特丁硫磷亚砜残留量[J].山东化工,2016,45(14):57-58.Zhang QY,Lin XX,Liao JY,et al.Determination of terbutenol sulfone and tert-butyl sulfoxide residues in vegetables and fruits by gas chromatography[J].Shandong Chem Ind,2016,45(14):57-58.
[11]马杰,李青,白梅,等.QuEChERS前处理技术与在线凝胶渗透色谱-气相色谱质谱联用法测定蔬菜水果中20种农药残留[J].食品安全质量检测学报,2016,7(1):20-26.Ma J,Li Q,Bai M,et al.Determination of 20 pesticide residues in vegetables and fruits by QuEChERS pretreatment and on-line gel permeation chromatography-gas chromatography-mass spectrometry[J].JFood Saf Qual,2016,7(1):20-26.
[12]田海,谭辉华,李雪生,等.分散液相微萃取-气相色谱法快速测定甘蔗中特丁硫磷残留[J].现代农药,2012,11(2):43-46.Tian H,Tan HH,Li XS,et al.Rapid determination of tetrathiophos residues in sugarcane by dispersive liquid phase microextraction-gas chromatography[J].Mod Agrochem,2012,11(2):43-46.
[13]李俊,蔡涛,周雪丽,等.气相色谱-三重四级杆质谱法同时测定农药中32种隐性添加成分[J].食品安全质量检测学报,2018,7(9):3219-3225.Li J,Cai T,Zhou XL,et al.Simultaneous determination of 32 implicit additives in pesticides by gas chromatography-triple quadrupole mass spectrometry[J].J Food Saf Qual,2018,7(9):3219-3225.
[14]陈丽娥,董晓尉.气相色谱检测果蔬中有机磷农药残留方法[J].南方农业,2017,11(2):86-88.Chen LE,Dong XL.Determination of organophosphorus pesticide residues in fruits and vegetables by gas chromatography[J].South China Agric,2017,11(2):86-88.
[15]Catherine B,Choung,Ross V,et al.Toxicity of the insecticide terbufos,its oxidation metabolites,and the herbicide atrazine in binary mixtures to ceriodaphnia cf dubia[J].Arch Environ Contam Toxicol,2011,(60):417-425.