QuEChERS-气相色谱法快速测定蔬菜中的咪鲜胺及2,4,6-三氯苯酚残留量
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摘要
建立了QuEChERS-气相色谱快速测定蔬菜中咪鲜胺及其代谢物2,4,6-三氯苯酚残留量的方法。样品经乙酸酸化乙腈提取后,以无水硫酸镁和N-丙基乙二胺(PSA)净化,并利用气相色谱进行检测。结果表明,在最佳条件下,咪鲜胺及其代谢物2,4,6-三氯苯酚分别在0.005～1.000和0.002～1.000μg/mL范围内线性关系良好,相关系数分别为0.998 6和0.999 3,检出限分别为0.001 0和0.000 6 mg/kg;在0.02、0.10、0.50μg/mL 3个添加水平下回收率分别为92.1%～107.9%和91.4%～105.7%,相对标准偏差分别为2.4%～10.4%和2.6%～11.3%。该方法具有快速、便捷、安全、清洁和成本低等特点,可用于蔬菜中咪鲜胺及其代谢物2,4,6-三氯苯酚残留的快速测定。
To developed a rapid method for the determination of residues of prochloraz and its metabolite 2,4,6-trichlorophenol in vegetables by QuEChERS and gas chromatography(GC). The samples were extracted with acetonitrile-acetic acid, purified by PSA,and determined by GC. The results showed that prochloraz and its metabolite 2,4,6-trichlorophenol had a good linearity in the range of 0.005～1.000 μg/mL and 0.002～1.000 μg/mL, the correlation were 0.998 6 and 0.999 3 under the optimal conditions. The limit of detection for prochloraz and its metabolite 2,4,6-trichlorophenol were 0.001 0 mg/kg and 0.000 6mg/kg, respectively. Their average recoveries at spiked levels of 0.01, 0.10 and 0.50 μg/mL were 92.1%～107.9% and 91.4%～105.7% with relative standard deviations of 2.4%～10.4% and 2.6%～11.3%, respectively. This method was simple, efficient,quick, convenient, safe, clean, low-cost, and can be suitable for the analysis of prochloraz and 2,4,6-trichlorophenol residues in fruit vegetables.
To developed a rapid method for the determination of residues of prochloraz and its metabolite 2,4,6-trichlorophenol in vegetables by QuEChERS and gas chromatography(GC). The samples were extracted with acetonitrile-acetic acid, purified by PSA,and determined by GC. The results showed that prochloraz and its metabolite 2,4,6-trichlorophenol had a good linearity in the range of 0.005～1.000 μg/mL and 0.002～1.000 μg/mL, the correlation were 0.998 6 and 0.999 3 under the optimal conditions. The limit of detection for prochloraz and its metabolite 2,4,6-trichlorophenol were 0.001 0 mg/kg and 0.000 6mg/kg, respectively. Their average recoveries at spiked levels of 0.01, 0.10 and 0.50 μg/mL were 92.1%～107.9% and 91.4%～105.7% with relative standard deviations of 2.4%～10.4% and 2.6%～11.3%, respectively. This method was simple, efficient,quick, convenient, safe, clean, low-cost, and can be suitable for the analysis of prochloraz and 2,4,6-trichlorophenol residues in fruit vegetables.
引文
[1] DE PAOLI M,BARBINA M T,DAMIANO V,et al. Simplified determination of combined residues of prochloraz and its metabolites in vegetable, fruit and wheat samples by gas chromatography[J].Journal of Chromatography A,1997,765(1):127-131.
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[3] WIESE F W,CHANG H C,LLOYD R V,et al. Peroxidase-catalyzed oxidation of 2,4,6-trichlorophenol[J].Archives of Environmental Contamination and Toxicology,1998,34(3):217-222.
[4] POLESE L,JARDIM E F G,NAVICKIENE S,et al. Prochloraz residue levels in ginger submitted to sportak 450 CE postharvest treatment[J].Eclética Química,2006,31(2):59-62.
[5]王建芳,李斌,赵彤,等.QuEChERS-高效液相色谱法同时检测茶鲜叶和乌龙茶中4种农药残留[J].食品科技,2017(8):306-313.
[6] CENGIZ M F,ERLER F,BILGIN A K,et al. Rapid and sensitive determination of the prochloraz residues in the cultivated mushroom,Agaricus bisporus(Lange)Imbach[J].Analytical Methods,2014,6(6):1970-1976.
[7]贾巧莉,王明强.超高效液相色谱法测定水果中咪鲜胺残留量[J].中国酿造,2015,34(9):145-148.
[8]卢俊文,李蓉,杨芳,等.气相色谱-串联质谱法快速测定水果中咪鲜胺及其代谢物2,4,6-三氯苯酚的残留量[J].食品科学,2015(12):213-217.
[9] BLASCO C,PIC魷Y,MANES J,et al. Determination of fungicide residues in fruits and vegetables by liquid chromatographyatmospheric pressure chemical ionization mass spectrometry[J].Journal of Chromatography A,2002,947(2):227-235.
[10] ZHAO P,CAO L,MA D,et al. Translocation,distribution and degradation of prochloraz-loaded mesoporous silica nanoparticles in cucumber plants[J].Nanoscale,2018,41(10):1798-1806.
[11]袁小雅,彭梓,周慧平,等.香蕉中咪鲜胺的消解动态及安全性评价[J].食品安全质量检测学报,2016(1):209-214.
[12]程莉,董丰收,刘新刚,等.QuEChERS-超高效液相色谱-串联质谱方法快速测定小麦中的咪鲜胺残留[J].农药学学报,2009,11(3):357-361.
[13]柳训才,陈平,程运斌,等.油菜体内及土壤中咪鲜胺的残留检测与消解动态[J].中国油料作物学报,2006,28(3):354-357.
[14]虞淼,梁赤周,唐芬芬,等.HPLC/MS/MS测定铁皮石斛中咪鲜胺残留[J].农药科学与管理,2016(7):34-37.
[15]王燕,王春伟,高洁,等.咪鲜胺在人参和土壤中的残留动态及安全性评价[J].东北农业大学学报,2014,45(3):25-30.
[2] H魻LLRIGL-ROSTA A,KREUZIG R, BAHADIR M. Investigations on the metabolic fate of prochloraz in soil under field and laboratory conditions[J].Pest Management Science,1999,55(5):531-538.
[3] WIESE F W,CHANG H C,LLOYD R V,et al. Peroxidase-catalyzed oxidation of 2,4,6-trichlorophenol[J].Archives of Environmental Contamination and Toxicology,1998,34(3):217-222.
[4] POLESE L,JARDIM E F G,NAVICKIENE S,et al. Prochloraz residue levels in ginger submitted to sportak 450 CE postharvest treatment[J].Eclética Química,2006,31(2):59-62.
[5]王建芳,李斌,赵彤,等.QuEChERS-高效液相色谱法同时检测茶鲜叶和乌龙茶中4种农药残留[J].食品科技,2017(8):306-313.
[6] CENGIZ M F,ERLER F,BILGIN A K,et al. Rapid and sensitive determination of the prochloraz residues in the cultivated mushroom,Agaricus bisporus(Lange)Imbach[J].Analytical Methods,2014,6(6):1970-1976.
[7]贾巧莉,王明强.超高效液相色谱法测定水果中咪鲜胺残留量[J].中国酿造,2015,34(9):145-148.
[8]卢俊文,李蓉,杨芳,等.气相色谱-串联质谱法快速测定水果中咪鲜胺及其代谢物2,4,6-三氯苯酚的残留量[J].食品科学,2015(12):213-217.
[9] BLASCO C,PIC魷Y,MANES J,et al. Determination of fungicide residues in fruits and vegetables by liquid chromatographyatmospheric pressure chemical ionization mass spectrometry[J].Journal of Chromatography A,2002,947(2):227-235.
[10] ZHAO P,CAO L,MA D,et al. Translocation,distribution and degradation of prochloraz-loaded mesoporous silica nanoparticles in cucumber plants[J].Nanoscale,2018,41(10):1798-1806.
[11]袁小雅,彭梓,周慧平,等.香蕉中咪鲜胺的消解动态及安全性评价[J].食品安全质量检测学报,2016(1):209-214.
[12]程莉,董丰收,刘新刚,等.QuEChERS-超高效液相色谱-串联质谱方法快速测定小麦中的咪鲜胺残留[J].农药学学报,2009,11(3):357-361.
[13]柳训才,陈平,程运斌,等.油菜体内及土壤中咪鲜胺的残留检测与消解动态[J].中国油料作物学报,2006,28(3):354-357.
[14]虞淼,梁赤周,唐芬芬,等.HPLC/MS/MS测定铁皮石斛中咪鲜胺残留[J].农药科学与管理,2016(7):34-37.
[15]王燕,王春伟,高洁,等.咪鲜胺在人参和土壤中的残留动态及安全性评价[J].东北农业大学学报,2014,45(3):25-30.