QuEChERS-气相色谱-电子捕获检测器监测浆果类水果常用的5种菊酯类农药残留
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摘要
目的建立一种利用QuEChERS提取法对浆果类水果进行提取、净化前处理,气相色谱-电子捕获检测器检测5种常用菊酯类农药的分析方法。方法浆果类水果均质后,用乙腈进行提取,提取液经QuEChERS提取法净化后,氮吹至近干,丙酮定容至1mL,0.22μm滤膜过滤后,上气相色谱仪,电子捕获检测器定量检测。结果 5种常用菊酯类农药质量浓度在0.02～5.0μg·mL-1范围内,具有良好的线性,相关系数(R2)均大于0.995;检出限在0.004～0.006mg·kg-1之间;加标回收率在84.5%～108.2%之间;重复性与精密度相对标准偏差(n=6)均在5.0%以内。结论该方法具有检出限低,检测结果准确,前处理简单等优点,适用于浆果类水果中菊酯类农药的检测。
OBJECTIVE A QuEChERS extraction method was established to extract and purify berry fruits and gas chromatography-electron capture detector(GC-ECD) was developed to detect five kinds of pyrethroid pesticides. METHOD Berry fruits samples were homogenized and extracted by acetonitrile, then purified by QuEChERS method. The purified solution was blown nearly dry by nitrogen, then fixed to 1 mL by acetone. After filtered by0.22μm filter membrane, samples were detected quantitatively by ECD. RESULT The concentration of 5 pyrethroid pesticides residues had good linear relationships in the range 0.02 ～5.0μg·m L-1, with correlation coefficients(R2)were all above 0.995; Detection limits were in the range 0.004 ～0.006 mg·kg-1.The recoveries were ranged from84.5%～108.2%. The RSD of reproducibility and precision were all below 5.0%(n=6). CONCLUSION This method has the advantages of low detection limit, accurate detection result and simple pretreatment, which is suitable for the detection of pyrethroids in berry fruits.
OBJECTIVE A QuEChERS extraction method was established to extract and purify berry fruits and gas chromatography-electron capture detector(GC-ECD) was developed to detect five kinds of pyrethroid pesticides. METHOD Berry fruits samples were homogenized and extracted by acetonitrile, then purified by QuEChERS method. The purified solution was blown nearly dry by nitrogen, then fixed to 1 mL by acetone. After filtered by0.22μm filter membrane, samples were detected quantitatively by ECD. RESULT The concentration of 5 pyrethroid pesticides residues had good linear relationships in the range 0.02 ～5.0μg·m L-1, with correlation coefficients(R2)were all above 0.995; Detection limits were in the range 0.004 ～0.006 mg·kg-1.The recoveries were ranged from84.5%～108.2%. The RSD of reproducibility and precision were all below 5.0%(n=6). CONCLUSION This method has the advantages of low detection limit, accurate detection result and simple pretreatment, which is suitable for the detection of pyrethroids in berry fruits.
引文
[1]冯建永.农药残留分析检测技术的发展概况[J].山东工业技术,2018,32(7):233-236.
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[7]邹沫君,余敏灵,景赞,等. GC-MS测定川芎中3种菊酯类农药残留[J].食品工业,2018,32(6):277-280.
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[9]刘洪波,赵晓芳,石贵英,等.浊点萃取反萃取-气质联用测定金线莲中5种拟除虫菊酯类农药残留[J].中国中药杂志,2014,39(15):2859-2862.
[10]刘洪波.气质联用测定杭白菊等3种中药中5种拟除虫菊酯类农药残留[J].浙江农林大学学报,2015,32(1):110-115.
[11]王锦,刘世军,唐志书,等.气相色谱法检测大枣中联苯菊酯农药残留[J].陕西农业科学,2018,64(9):12-13.
[12]张朋杰,张宪臣,唐志书,等. QuEChERS-高效液相色谱-质谱/质谱法同时测定水产品中磺胺类和氯霉素类药物[J].食品安全质量检测学报,2018,9(20):5403-5409.
[13]胡秋辉,张昌娟,郑惠华,等.固相萃取-气相色谱-质谱联用法筛查食用菌中的农药残留[J].食品科学,2015,36(14):171-175.
[2]华乃震.拟除虫菊酯农药的进展和趋向[J].农药市场信息,2015,26(3):26-29.
[3]吴俊,郑翔,让蔚清. QuEChERS方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.
[4]任方方,唐雪明.氰基类拟除虫菊酯类农药检测研究进展[J].现代农业科技, 2014, 17(7):150-152.
[5]张立华,赵戈祎. GC-ECD检测茶叶中4种拟除虫菊酯类农药残留研究[J].山东化工,2016,45(17):69-74.
[6]王万成,柳敏. QuEChERS-气相色谱分析铁皮石斛中的6种有机磷农药残留[J].吉林农业,2017,36(12):70-71.
[7]邹沫君,余敏灵,景赞,等. GC-MS测定川芎中3种菊酯类农药残留[J].食品工业,2018,32(6):277-280.
[8]吴俊,郑翔,让蔚清. QuEChERS方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.
[9]刘洪波,赵晓芳,石贵英,等.浊点萃取反萃取-气质联用测定金线莲中5种拟除虫菊酯类农药残留[J].中国中药杂志,2014,39(15):2859-2862.
[10]刘洪波.气质联用测定杭白菊等3种中药中5种拟除虫菊酯类农药残留[J].浙江农林大学学报,2015,32(1):110-115.
[11]王锦,刘世军,唐志书,等.气相色谱法检测大枣中联苯菊酯农药残留[J].陕西农业科学,2018,64(9):12-13.
[12]张朋杰,张宪臣,唐志书,等. QuEChERS-高效液相色谱-质谱/质谱法同时测定水产品中磺胺类和氯霉素类药物[J].食品安全质量检测学报,2018,9(20):5403-5409.
[13]胡秋辉,张昌娟,郑惠华,等.固相萃取-气相色谱-质谱联用法筛查食用菌中的农药残留[J].食品科学,2015,36(14):171-175.
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