一种测定21种蔬菜中甲基异柳磷含量的方法
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摘要
本方法以21种蔬菜为检测对象,建立一种测定21种蔬菜中甲基异柳磷残留量的方法。样品经乙酸乙酯提取,无水硫酸干燥后,浓缩,经火焰光度检测器测定,供气相色谱分析。使用毛细管色谱柱DB-1701(30 m×320μm×0.25μm)进行分离,以保留时间定性,外标法定量。最终,由测定结果可知,本方法在浓度范围:0.020～0.2μg·mL~(-1)峰面积成良好的线性关系,相关系数R=0.9991;3个加标回收浓度为0.020、0.080、0.20μg,得到平均加标回收率为87.1%～97.7%;以3倍信噪比、基线噪声为2.0 pAos计算检出限为0.0029 mg·kg~(-1);相对标准偏差(RSD)为0.16%～1.44%。该方法操作简单、耗时短、能够准确定性定量、可靠,且抗干扰性好,可为21蔬菜中甲基异柳磷的检测提高效率,可作为一种高效的分析方法。
A method was developed for the determination of isoliphos-methyl residues in 21 vegetables.The sample was extracted with ethyl acetate,dried with anhydrous sulfuric acid,concentrated,determined by flame photometric detector and analyzed by gas chromatography.Capillary column DB-1701(30 m × 320 μm × 0.25 μm) was used for separation,and retention time was used for qualitative analysis and external standard method for quantitative analysis.Finally,the results showed that the peak area of the method was linear in the concentration range of 0.020～0.2 μg·mL~(-1).and the correlation coefficient was 0.9991.The concentration of 3 recoveries were 0.020,0.080 and 0.20 μg,respectively,and the average recoveries were 87.1%～ 97.7%,respectively.Using 3 times SNR and baseline noise as 2.0 pA·s,the detection limit was calculated as 0.0029 mg·kg~(-1); relative standard deviation(RSD) of 0.16%～1.44%.This method is simple,time-consuming,accurate,qualitative and quantitative,reliable,and anti-interference,it can improve the efficiency for the determination of methyl isofen in 21 vegetables,and can be used as an efficient analytical method.
A method was developed for the determination of isoliphos-methyl residues in 21 vegetables.The sample was extracted with ethyl acetate,dried with anhydrous sulfuric acid,concentrated,determined by flame photometric detector and analyzed by gas chromatography.Capillary column DB-1701(30 m × 320 μm × 0.25 μm) was used for separation,and retention time was used for qualitative analysis and external standard method for quantitative analysis.Finally,the results showed that the peak area of the method was linear in the concentration range of 0.020～0.2 μg·mL~(-1).and the correlation coefficient was 0.9991.The concentration of 3 recoveries were 0.020,0.080 and 0.20 μg,respectively,and the average recoveries were 87.1%～ 97.7%,respectively.Using 3 times SNR and baseline noise as 2.0 pA·s,the detection limit was calculated as 0.0029 mg·kg~(-1); relative standard deviation(RSD) of 0.16%～1.44%.This method is simple,time-consuming,accurate,qualitative and quantitative,reliable,and anti-interference,it can improve the efficiency for the determination of methyl isofen in 21 vegetables,and can be used as an efficient analytical method.
引文
[1]余霞奎,王晓娟.气相色谱法测定蔬菜水果中甲基异柳磷残留[J].安徽农学通报,2013,19(22):96-97.
[2]费仁雷,张滢,张化平,等.甲基异柳磷在土壤中的残留降解分析[J].安徽农学通报,2016,22(22):104-105.
[3]朱卫芳,汪滨,张建辉.蔬果中甲基异柳磷残留量检测方法研究[J].上海农业科技,2016(6):32,51.
[4]班秋丽,江露,汪善良.气相色谱法测定蔬菜中甲基异柳磷农药残留量不确定度分析[J].现代农业科技,2017(20):114-116,120.
[5]黄伟雄,邓峰,高燕红.食品中甲基异柳磷残留量测定方法的研究[J].中国食品卫生杂志,2001(4):19-20.
[6]国家卫生和计划生育委员会,农业部,国家食品药品监督管理总局.GB 2763-2016 食品安全国家标准食品中农药最大残留限量[S].北京:中国标准出版社,2016.
[7]中华人民共和国卫生部.GB/T 5009.144-2003 植物性食品中甲基异柳磷残留量的测定[S].北京:中国标准出版社,2003.
[8]中华人民共和国农业部.NYT 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].北京:农业出版社,2008.
[9]朱莉娅,韩宇,陈文,等.表面增强拉曼光谱快速检测西瓜中甲基异柳磷农药残留[J].食品工业科技,2017,38(20):288-291,322.
[10]朱莉娅,韩宇,陈文,等.西瓜中甲基异柳磷农药残留的表面增强拉曼光谱快速检测[J/OL].食品工业科技:1-11[2019-01-08].http://kns.cnki.net/kcms/detail/11.1759.TS.20170607.1741.054.html.
[11]刘晓锋,黄克建,罗正坚,等.甲基异柳磷的GC/MS检验及谱图解析[J].广西警官高等专科学校学报,2006(S1):16-17.
[12]王金略.气质联用仪测定蔬菜中的甲基异柳磷农药残留[J].中国农业信息,2016(19):125.
[2]费仁雷,张滢,张化平,等.甲基异柳磷在土壤中的残留降解分析[J].安徽农学通报,2016,22(22):104-105.
[3]朱卫芳,汪滨,张建辉.蔬果中甲基异柳磷残留量检测方法研究[J].上海农业科技,2016(6):32,51.
[4]班秋丽,江露,汪善良.气相色谱法测定蔬菜中甲基异柳磷农药残留量不确定度分析[J].现代农业科技,2017(20):114-116,120.
[5]黄伟雄,邓峰,高燕红.食品中甲基异柳磷残留量测定方法的研究[J].中国食品卫生杂志,2001(4):19-20.
[6]国家卫生和计划生育委员会,农业部,国家食品药品监督管理总局.GB 2763-2016 食品安全国家标准食品中农药最大残留限量[S].北京:中国标准出版社,2016.
[7]中华人民共和国卫生部.GB/T 5009.144-2003 植物性食品中甲基异柳磷残留量的测定[S].北京:中国标准出版社,2003.
[8]中华人民共和国农业部.NYT 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].北京:农业出版社,2008.
[9]朱莉娅,韩宇,陈文,等.表面增强拉曼光谱快速检测西瓜中甲基异柳磷农药残留[J].食品工业科技,2017,38(20):288-291,322.
[10]朱莉娅,韩宇,陈文,等.西瓜中甲基异柳磷农药残留的表面增强拉曼光谱快速检测[J/OL].食品工业科技:1-11[2019-01-08].http://kns.cnki.net/kcms/detail/11.1759.TS.20170607.1741.054.html.
[11]刘晓锋,黄克建,罗正坚,等.甲基异柳磷的GC/MS检验及谱图解析[J].广西警官高等专科学校学报,2006(S1):16-17.
[12]王金略.气质联用仪测定蔬菜中的甲基异柳磷农药残留[J].中国农业信息,2016(19):125.