快速溶剂萃取-气相色谱质谱法联用测定大米中6种甲氧基丙烯酸酯类杀菌剂残留
|
摘要
建立了快速溶剂萃取(APLE)-在线净化-气相色谱质谱法(GC/MS)检测大米中6种甲氧基丙烯酸酯类杀菌剂残留含量的方法。大米经硅藻土分散后,放入事先在萃取池底部装有无水硫酸镁(MgSO4)、乙二胺氮丙基硅烷(PSA)和C18的萃取池中,以乙腈为溶剂用快速溶剂萃取仪萃取并同时完成净化,以气相色谱质谱(GC/MS)定性定量检测。6种甲氧基丙烯酸酯类杀菌剂在0.05～1μg/mL浓度范围内呈线性,相关系数为0.9992～1.0000。在空白样品中,添加6种甲氧基丙烯酸酯类杀菌剂的回收率为84.7～95.6%,精密度(RSD)为0.22～3.69%,各组分检出限均在0.002～0.022μg/mL之间(S/N=3),定量限在0.007～0.246μg/mL之间(S/N=10)。该方法自动化程度高,快速高效,满足测定大米中甲氧基丙烯酸酯类杀菌剂的检测要求。
The rice samples were dispersed with diatomite and then put into the extraction pools with pre placed anhydrous magnesium sulfate,PSA and C18 at the bottoms.six strobilurin fungicides were extracted with acetonitrile and purified in situ by the accelerated solvent extractor,and then analyzed by GC/MS.The results showed a good linear relationship for all the analytes in the range of 0.05—1μg/mL with the correlation coefficients of 0.9992—1.000.The mean recoveries of strobilurin fungicides in the spiked rice samples were within 84.7%—95.6% and the relative standard deviations were in the range of0.22%—3.69%(n=3)at three spiked levels(0.05,0.1 and 0.2 mg/kg).The limits of detection were within 0.002—0.022μg/mL(S/N=3)while the limits of quantitation were in the range of 0.007—0.246μg/mL(S/N=10).The method is of high-efficiency and very applicable in real rice analysis.
The rice samples were dispersed with diatomite and then put into the extraction pools with pre placed anhydrous magnesium sulfate,PSA and C18 at the bottoms.six strobilurin fungicides were extracted with acetonitrile and purified in situ by the accelerated solvent extractor,and then analyzed by GC/MS.The results showed a good linear relationship for all the analytes in the range of 0.05—1μg/mL with the correlation coefficients of 0.9992—1.000.The mean recoveries of strobilurin fungicides in the spiked rice samples were within 84.7%—95.6% and the relative standard deviations were in the range of0.22%—3.69%(n=3)at three spiked levels(0.05,0.1 and 0.2 mg/kg).The limits of detection were within 0.002—0.022μg/mL(S/N=3)while the limits of quantitation were in the range of 0.007—0.246μg/mL(S/N=10).The method is of high-efficiency and very applicable in real rice analysis.
引文
[1]薄海波,王金花,郭春海,等.气相色谱/串联质谱法测定食品中氧基丙烯酸酯类杀菌剂残留[J].分析化学研究报告,2008,36(11):1471-1475.
[2]薄海波.固相萃取-气相色谱/质谱法分析水果和蔬菜中残留的嘧菌酯[J].色谱,2007,25(6):898-901.
[3]陶凌云.固相萃取-气相色谱质谱法同时测定水果蔬菜中13种三唑类杀菌剂[J].中国卫生检验杂志,2017(23):3385-3387.
[4]雒丽丽,薄海波,毕阳,等.超高效液相色谱法测定水果和饮料中残留的氟嘧菌酯和嘧螨酯[J].色谱,2009,27(2):201-205.
[5]张育乐,黄超群,朱晓雨,等.固相萃取-液相色谱-串联质谱法测定中药材中7种甲氧基丙烯酸酯类杀菌剂的残留量[J].色谱,2013,31(3):264-269.
[6]de La Cal A,Eljarrat E,BarcelóD.Determination of 39polybrominateddiphenyl ether congeners in sediment samples using fast selective pressurized liquid extraction and purification[J].Journal of Chromatography A,2003,1021(1):165-173.
[7]Berset J D,Ejem M,Holzer R,et al.Comparison of different drying,extraction and detection techniques for the determination of priority polycyclic aromatic hydrocarbons in background contaminated soil samples[J].AnalyticaChimicaActa,1999,383(3):263-275.
[8]Flotron V,Houessou J,Bosio A,et al.Rapid determination of polycyclic aromatic hydrocarbons in sewage sludges using microwave-assisted solvent extraction.Comparison with other extraction methods[J].Journal of Chromatography A,2003,999(1):175-184.
[9]Test Methods for Evaluating Solid Waste,Method 3545.USEPASW-846,Update III,3rd ed.,U.S.GPO,Washington,DC,1995.
[10]金党琴,丁邦东,孔勇.快速溶剂萃取高效液相色谱法测定蔬菜中噻虫嗪残留量[J].分析仪器,2014,(2):69-72.
[11]王云凤,葛宝坤,高建会,等.液相色谱-质谱法测定果蔬中8种甲氧基丙烯酸酯类杀菌剂残留量[J].食品研究与开发,2009,30(4):130-133.
[12]Schurek J,Vaclavik L,Hooijerink H D,et al.Control of strobilurin fungicides in wheat using direct analysis in real time accurate time-of-flight and desorption electrospray ionization linear ion trap mass spectrometry[J].Analytical Chemistry,2008,80(24):9567-9575.
[13]Zhang F,Wang L,Zhou L,et al.Residue dynamics of pyraclostrobin in peanut and field soil by QuEChERSand LC-MS/MS[J].Ecotoxicology&Environmental Safety,2012,78(2):116-122.
[14]Banerjee K,Oulkar D P,Paul S B.Multiresidue Determination and Uncertainty Analysis of 87Pesticides in Mango by Liquid Chromatography-Tandem Mass Spectrometry[J].J Agric Food Chem,2009,57(10):4068-4078.
[15]吴加伦,王怀昌,武秀停,等.嘧菌酯在人参和西洋参中的残留监测及其膳食风险评估[J].农药学学报,2012,14(1):67-73.
[2]薄海波.固相萃取-气相色谱/质谱法分析水果和蔬菜中残留的嘧菌酯[J].色谱,2007,25(6):898-901.
[3]陶凌云.固相萃取-气相色谱质谱法同时测定水果蔬菜中13种三唑类杀菌剂[J].中国卫生检验杂志,2017(23):3385-3387.
[4]雒丽丽,薄海波,毕阳,等.超高效液相色谱法测定水果和饮料中残留的氟嘧菌酯和嘧螨酯[J].色谱,2009,27(2):201-205.
[5]张育乐,黄超群,朱晓雨,等.固相萃取-液相色谱-串联质谱法测定中药材中7种甲氧基丙烯酸酯类杀菌剂的残留量[J].色谱,2013,31(3):264-269.
[6]de La Cal A,Eljarrat E,BarcelóD.Determination of 39polybrominateddiphenyl ether congeners in sediment samples using fast selective pressurized liquid extraction and purification[J].Journal of Chromatography A,2003,1021(1):165-173.
[7]Berset J D,Ejem M,Holzer R,et al.Comparison of different drying,extraction and detection techniques for the determination of priority polycyclic aromatic hydrocarbons in background contaminated soil samples[J].AnalyticaChimicaActa,1999,383(3):263-275.
[8]Flotron V,Houessou J,Bosio A,et al.Rapid determination of polycyclic aromatic hydrocarbons in sewage sludges using microwave-assisted solvent extraction.Comparison with other extraction methods[J].Journal of Chromatography A,2003,999(1):175-184.
[9]Test Methods for Evaluating Solid Waste,Method 3545.USEPASW-846,Update III,3rd ed.,U.S.GPO,Washington,DC,1995.
[10]金党琴,丁邦东,孔勇.快速溶剂萃取高效液相色谱法测定蔬菜中噻虫嗪残留量[J].分析仪器,2014,(2):69-72.
[11]王云凤,葛宝坤,高建会,等.液相色谱-质谱法测定果蔬中8种甲氧基丙烯酸酯类杀菌剂残留量[J].食品研究与开发,2009,30(4):130-133.
[12]Schurek J,Vaclavik L,Hooijerink H D,et al.Control of strobilurin fungicides in wheat using direct analysis in real time accurate time-of-flight and desorption electrospray ionization linear ion trap mass spectrometry[J].Analytical Chemistry,2008,80(24):9567-9575.
[13]Zhang F,Wang L,Zhou L,et al.Residue dynamics of pyraclostrobin in peanut and field soil by QuEChERSand LC-MS/MS[J].Ecotoxicology&Environmental Safety,2012,78(2):116-122.
[14]Banerjee K,Oulkar D P,Paul S B.Multiresidue Determination and Uncertainty Analysis of 87Pesticides in Mango by Liquid Chromatography-Tandem Mass Spectrometry[J].J Agric Food Chem,2009,57(10):4068-4078.
[15]吴加伦,王怀昌,武秀停,等.嘧菌酯在人参和西洋参中的残留监测及其膳食风险评估[J].农药学学报,2012,14(1):67-73.