茶基质对气相色谱法定量分析有机磷农药的影响
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摘要
选用茶叶、茶汤为基质,气相色谱法分析茶叶、茶汤对毒死蜱、甲基对硫磷、敌敌畏的基质效应。结果表明:优化色谱条件下,3种农药有较好分离效果和重现性。以不添加基质标准曲线与分别添加2种基质标准曲线的R~2值均大于0.99;同一种农药基质标准曲线斜率与纯溶剂标准曲线斜率之比得出,基质增强效应明显,茶叶茶汤对3种农药的基质效应为敌敌畏>甲基对硫磷>毒死蜱。基质对回收率有较大影响,以添加基质的标准曲线定量,3种农药3个加标水平的回收率为74.75%～113.20%;以不添加基质的标准曲线定量,3种农药3个加标水平的回收率为80.40%～133.80%,其中茶叶3种农药加标量为0.4 mg/kg时,3种农药的回收率均超过120%。RSD(相对标准偏差)在0.79%～6.57%之间,基质对RSD影响不明显。说明茶基质对低浓度3种农药具有明显基质增强效应,采用基质标准溶液的定量方式对低浓度水平有机磷农药的检测有较好准确度。
Tea and tea soup were used as matrix,the matrix effects of chlorpyrifos,methyl parathion and dichlorvos were analyzed by gas chromatography. The results were as follows:Under the optimized chromatographic conditions,the 3 pesticides had good separation effect and reproducibility. The R~2 values of standard curves without matrix addition and those with two matrix addition were both greater than 0.99.The ratio of the slope of the standard curve of the same pesticide matrix to that of the standard curve of the pure solvent showed that the enhancement effect of the matrix was obvious. The enhancement effect of matrix on 3 pesticides was dichlorvos>methyl parathion>chlorpyrifos. Matrix had great influence on recovery rate,the recoveries of three standard levels of pesticides in tea were 74.75%～113.20% based on the standard curve of adding substrates,and 80.40%～133.80% based on the standard curve of not adding substrates,when the additive scalar in the tea was 0.4 mg/kg,the recovery rates of the 3 pesticides were all greater than 120%. The RSD value was 0.79%～6.57%,and the matrix had no obvious effect on RSD. It showed that tea had obvious matrix enhancement effect on the low concentration of 3 kinds of pesticide,calibration method using matrix standard curve had good accuracy for the detection of low concentration organophosphorus pesticides.
Tea and tea soup were used as matrix,the matrix effects of chlorpyrifos,methyl parathion and dichlorvos were analyzed by gas chromatography. The results were as follows:Under the optimized chromatographic conditions,the 3 pesticides had good separation effect and reproducibility. The R~2 values of standard curves without matrix addition and those with two matrix addition were both greater than 0.99.The ratio of the slope of the standard curve of the same pesticide matrix to that of the standard curve of the pure solvent showed that the enhancement effect of the matrix was obvious. The enhancement effect of matrix on 3 pesticides was dichlorvos>methyl parathion>chlorpyrifos. Matrix had great influence on recovery rate,the recoveries of three standard levels of pesticides in tea were 74.75%～113.20% based on the standard curve of adding substrates,and 80.40%～133.80% based on the standard curve of not adding substrates,when the additive scalar in the tea was 0.4 mg/kg,the recovery rates of the 3 pesticides were all greater than 120%. The RSD value was 0.79%～6.57%,and the matrix had no obvious effect on RSD. It showed that tea had obvious matrix enhancement effect on the low concentration of 3 kinds of pesticide,calibration method using matrix standard curve had good accuracy for the detection of low concentration organophosphorus pesticides.
引文
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[6]江波,徐昆龙,田洋,等.晒青茶叶和烘青茶叶成分比较研究[J].云南农业大学学报,2010,25(3):409-412.
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[11]朱作为,张文中,陈沙,等.气相色谱-三重四极杆串联质谱法测定大米、韭菜、茶叶3种基质中51种农药残留的研究[J].食品安全质量检测学报,2018,9(6):1297-1300.
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[13]高艺羡,陈萍虹,聂丹丹.气相色谱-串联质谱双内标法测定茶叶中53种农药残留[J].色谱,2018,36(6):531.
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[15]胡雪艳,彭涛,陈辉,等.茶叶中10种农药残留的液相色谱-串联质谱法和气相色谱-串联质谱法测定[J].食品工业科技,2018,39(17):240-247.
[16]钱承敬,史晓梅,谢云峰,等.气相色谱-串联质谱法测定茶叶茶汤中多种农药残留量[J].食品安全质量检测学报,2017,8(8):3218.
[17]中华人民共和国农业部.NY/T 761-2008.蔬菜和水果中有机磷农药残留检测方法[S].北京:中国农业出版社,2008.
[18]董新凤,李丽敏,郭爱静,等.固相萃取-气相色谱双检测器法测定蔬菜中26种有机磷农药残留量[J].中国食品卫生杂志,2012,24(1):41-42.
[19]吴晖,朱珍,风华亮.蔬菜中11种有机磷农药残留的气相色谱检测及其对蔬菜基质的影响[J].食品科学,2011,32(6):198-203.
[20]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 27404-2008.实验室质量控制规范食品理化检测[S].北京:中国标准出版社,2008.
[2]刘艳芳,王胜鹏.中国茶叶安全现状及产地溯源技术研究[J].湖北农业科学,2014,5(24):5914.
[3]Zhu X Q,Zhao W,Chen T L.Modified QuEChERS method with gas chromatography-flame photometric detection for the determination of 5 organophosphorus pesticides in tea[J].Journal of Analytical Science,2018(2):176-180.
[4]Cho S K,AbdElaty A M,Rahman M M,et al.Simultaneous multi-determination and transfer of eight pesticide residues from green tealeaves to infusion using gas chromatography[J].Food Chemistry,2014,165(3):532-539.
[5]Chen H P,Yin P,Wang Q H,et al.A modified QuEChERS sample preparation method for the analysis of 70 pesticide residues in tea using gas chromatography-tandem mass spectrometry[J].Food Anal Methods,2014,7:1577-1587.
[6]江波,徐昆龙,田洋,等.晒青茶叶和烘青茶叶成分比较研究[J].云南农业大学学报,2010,25(3):409-412.
[7]黄田田,汤桦,董晓倩,等.多壁碳纳米管QuEChERS-气相色谱法测定茶叶中23种有机磷农药残留量[J].食品科学,2018,39(6):315-321.
[8]刘腾飞,董明辉,杨代凤,等.茶叶质量安全主要化学影响因素分析方法研究进展[J].食品科学,2018,39(9):310-318.
[9]刘莉,袁名安,盛仙俏,等.基质效应对黄瓜中4种有机磷农药残留检测的影响[J].浙江农业学报,2014,26(6):1564-1567.
[10]杨旭,汤佳峰,巢文军.基质效应对有机磷农药测定的影响及其解决方法[J].分析测试学报,2009,28(12):1368-1369.
[11]朱作为,张文中,陈沙,等.气相色谱-三重四极杆串联质谱法测定大米、韭菜、茶叶3种基质中51种农药残留的研究[J].食品安全质量检测学报,2018,9(6):1297-1300.
[12]刘腾飞,董明辉,张丽,等.茶鲜叶中有机磷农药残留分析[J].食品科学技术学报,2016,34(4):66-67.
[13]高艺羡,陈萍虹,聂丹丹.气相色谱-串联质谱双内标法测定茶叶中53种农药残留[J].色谱,2018,36(6):531.
[14]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 23776-2018.茶叶感官评审方法[S].北京:中国标准出版社,2018.
[15]胡雪艳,彭涛,陈辉,等.茶叶中10种农药残留的液相色谱-串联质谱法和气相色谱-串联质谱法测定[J].食品工业科技,2018,39(17):240-247.
[16]钱承敬,史晓梅,谢云峰,等.气相色谱-串联质谱法测定茶叶茶汤中多种农药残留量[J].食品安全质量检测学报,2017,8(8):3218.
[17]中华人民共和国农业部.NY/T 761-2008.蔬菜和水果中有机磷农药残留检测方法[S].北京:中国农业出版社,2008.
[18]董新凤,李丽敏,郭爱静,等.固相萃取-气相色谱双检测器法测定蔬菜中26种有机磷农药残留量[J].中国食品卫生杂志,2012,24(1):41-42.
[19]吴晖,朱珍,风华亮.蔬菜中11种有机磷农药残留的气相色谱检测及其对蔬菜基质的影响[J].食品科学,2011,32(6):198-203.
[20]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 27404-2008.实验室质量控制规范食品理化检测[S].北京:中国标准出版社,2008.