一种利用QuEChERS-GC/MS测定苹果种植土壤中5种常见菊酯类农药的方法研究
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摘要
实验建立利用QuEChERS提取苹果种植土壤中的5种菊酯类农药(甲氰菊酯、联苯菊酯、高效氯氟氰菊酯、氯菊酯、氰戊菊酯),气相色谱-质谱法定性定量检测的分析方法。苹果种植土壤样品用乙腈:冰乙酸(9:1,V/V)进行超声提取,QuEChERS方法进行净化处理,净化后的溶液用氮吹仪吹干,残渣用丙酮溶解定容至1 mL,0.45μm滤膜过滤,GC-MS仪定性定量检测。结果表明:5种菊酯类农药在0.1～50.0μg/mL范围内线性关系良好,r2均大于0.995;检出限在0.008～0.02 mg/kg之间,加标回收率范围为80.6%～106.7%;精密度相对标准偏差在1.8%～2.8%之间,重复性相对标准偏差在3.5%～4.6%之间。实验证明该方法具有前处理简单、检测速度快、灵敏度高、检测结果准确等优点。
A QuEChERS pr-treatment method for extracting 5 pyrethroid pesticide residues(fenpropathrin,bifenthrin, lambda-cyhalothrin, permethrin and fenvalerate) in planting soil of apple and GC/MS method for determination quantitatively was established. Planting soil of apple samples were ultrasoned and extracted by acetonitrile:glacial acetic acid(9:1,V/V), QuEChERS was used for sample purifying. Purification solution was firstly concentrated to dry under nitrogen, then the residue was dilute with acetone to 1 mL, filtered with0.45 μm filter membrane and detected qualitatively and quantitatively by GC/MS. It was showed that concentration of 5 pyrethroid pesticide showed good linear relationships in the range 0.1-50.0 μg/mL, the correlation coefficients were all above 0.995. The detection limits were bewteen 0.008-0.02 mg/kg and the recoveries were ranged from 80.6%-106.7%. RSD of precision were ranged from 1.8%-2.8%, Repeatability of the relative standard deviation(RSD) of 6 pesticide residues were 3.5%-4.6%. This method was proved to be simple and quick pre-treated with high sensitivity and accuracy.
A QuEChERS pr-treatment method for extracting 5 pyrethroid pesticide residues(fenpropathrin,bifenthrin, lambda-cyhalothrin, permethrin and fenvalerate) in planting soil of apple and GC/MS method for determination quantitatively was established. Planting soil of apple samples were ultrasoned and extracted by acetonitrile:glacial acetic acid(9:1,V/V), QuEChERS was used for sample purifying. Purification solution was firstly concentrated to dry under nitrogen, then the residue was dilute with acetone to 1 mL, filtered with0.45 μm filter membrane and detected qualitatively and quantitatively by GC/MS. It was showed that concentration of 5 pyrethroid pesticide showed good linear relationships in the range 0.1-50.0 μg/mL, the correlation coefficients were all above 0.995. The detection limits were bewteen 0.008-0.02 mg/kg and the recoveries were ranged from 80.6%-106.7%. RSD of precision were ranged from 1.8%-2.8%, Repeatability of the relative standard deviation(RSD) of 6 pesticide residues were 3.5%-4.6%. This method was proved to be simple and quick pre-treated with high sensitivity and accuracy.
引文
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[2]梁茹晶,宋雪英,宋晗,等.氟氯氰菊酯、溴氰菊酯和联苯菊酯对赤子爱胜蚓的急性毒性[J].沈阳药科大学学报, 2016,33(11):901-907.
[3]于玲,董丽丽.分散固相萃取-超声辅助分散液液微萃取/高效液相色谱法测定土壤中溴氰菊酯残留[J].分析科学学报,2016, 32(2):218-222.
[4]王世英,黄日林,李梓豪,等.联苯菊酯在甘蓝及土壤中的消解动态[J].华南农业大学学报, 2016, 37(3):82-85.
[5]李劭彤,李朝阳,李巧玲,等.甲氰菊酯微生物降解的研究进展[J].江苏农业科学, 2015, 43(11):17-20.
[6]吴俊,郑翔,让蔚清. QuEchERS法在食品农药残留检测中的应用前景[J].实用预防医学, 2010, 17(3):619-621.
[7]陈姣姣,张静,吴思卓,等.气相色谱法测定苹果和土壤中的高效氯氟氰菊酯[J].色谱, 2016, 34(10):1005-1010.
[8]王璞,何明远,刘勇,等. 4种拟除虫菊酯类农药在苎麻与土壤中的残留消解动态及最终残留研究[J].湖南农业科学,2013, 43(3):85-89.
[9]刘丽,张琦,王海雁,等.串联双柱固相萃取-气相色谱-串联质谱法检测茶叶中拟除虫菊酯[J].色谱, 2017, 35(8):860-866.
[10]秦伟瀚,阳勇,师萱,等.基质分散固相萃取法同时检测13种不同产地昆明山海棠中有机磷和拟除虫菊酯类农药残留[J].中国医院药学杂志, 2017, 37(7):613-616.
[11]胡西洲,程运斌,胡定金. QuEchERS法测定蔬菜中有机磷类农药多残留分析[J].中国测试技术, 2006, 32(3):132-134.
[12]张爱娟,梁林,翟淑华,等.超高效液相色谱串联质谱法检测辣椒及土壤中啶氧菌酯的残留[J].农药科学与管理,2016(10):40-43.
[13]江泽军,张鹏,李永飞,等.分散固相萃取-高效液相色谱-串联质谱法测定水稻和土壤中的福美双与甲霜灵残留[J].农药学学报, 2015, 17(3):313-320.