气相色谱-质谱联用法测定茶叶中21种农药残留
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摘要
该实验建立了茶叶中21种农药残留的气相色谱-质谱(GC-MS)多反应监测模式(MRM)定性、定量分析检测方法,探讨不同提取方法、提取溶剂、浓缩方式等试验因素对茶叶农药多残留测定结果的影响。结果表明,以正己烷-丙酮(1∶1,V/V)混合溶剂超声提取、氮吹浓缩,用气相色谱-质谱法对茶叶样品中21种农药进行定性定量检测,21种农药在0.05～1.00μg/mL范围内呈良好的线性关系,相关系数(R~2)为0.9980～0.9999。在茶叶样品中分别添加质量浓度0.05mg/kg、0.20mg/kg、0.40mg/kg的农药组分,平均回收率为83.46%～92.13%,相对标准偏差(RSD)为4.88%～8.51%,检出限为0.0027～0.0219mg/kg,该方法具有前处理简便快捷、灵敏度高、成本低等优点,在实际茶叶农药残留检测中得到了广泛应用,能满足日常的茶叶农药残留检测。
A determination method for qualitative and quantitative analysis of 21 kinds of pesticides residues in tea was developed by GC-MS combined with MRM mode. The effects of different extraction methods, solvents and concentration methods on the determination of pesticide residues in tea were investigated. Results showed that using ultrasonic extraction of n-hexane+acetone(1∶1, V/V) mixed solvent and concentration by nitrogen blowing, the 21 kinds of pesticides were qualitatively and quantitatively detected, and the pesticides were in good linearity in the concentrations of 0.05-1.00 μg/ml(correlation coefficient R~2 were 0.998 0-0.9999). After adding the spiked levels of 0.05 mg/kg, 0.2 mg/kg, 0.4 mg/kg, the average recoveries varied from 83.46% to 92.13%, and the relative standard deviations(RSD) ranged from 4.88% to 8.51%, and the limit of detection was 0.002 7-0.0219 mg/kg. The method had the advantages of simple pretreatment, high sensitivity, high accuracy and low cost, the method was widely used in the practical detection of pesticide residues in tea, which met the requirements daily detection of pesticide residues in tea.
A determination method for qualitative and quantitative analysis of 21 kinds of pesticides residues in tea was developed by GC-MS combined with MRM mode. The effects of different extraction methods, solvents and concentration methods on the determination of pesticide residues in tea were investigated. Results showed that using ultrasonic extraction of n-hexane+acetone(1∶1, V/V) mixed solvent and concentration by nitrogen blowing, the 21 kinds of pesticides were qualitatively and quantitatively detected, and the pesticides were in good linearity in the concentrations of 0.05-1.00 μg/ml(correlation coefficient R~2 were 0.998 0-0.9999). After adding the spiked levels of 0.05 mg/kg, 0.2 mg/kg, 0.4 mg/kg, the average recoveries varied from 83.46% to 92.13%, and the relative standard deviations(RSD) ranged from 4.88% to 8.51%, and the limit of detection was 0.002 7-0.0219 mg/kg. The method had the advantages of simple pretreatment, high sensitivity, high accuracy and low cost, the method was widely used in the practical detection of pesticide residues in tea, which met the requirements daily detection of pesticide residues in tea.
引文
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[15]曹艳平,姜大峰,李凤华,等.气相色谱-三重四极杆质谱同位素内标法测定鱼样中20种多氯联苯[J].色谱,2018,36(7):685-692.
[16]刘家曾,宋宁慧,王艺璇,等.基质固相分散-气相色谱/质谱联用技术测定茶叶中8种农药残留[J].分析科学学报,2018,34(3):337-341.
[17]刘慧,徐怡,游燕,等.气相色谱-质谱联用法测定茶叶中17种农药残留[J].广州化工,2017,45(18):87-89.
[18]李玮,贾彦博,林伟杰,等.分散固相萃取净化-气相色谱-质谱联用法测定茶叶中7种杀螨杀虫类农药残留[J].食品安全质量检测学报,2017,8(9):3485-3490.
[19]高艺羡,陈萍虹,聂丹丹,等.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):531-540.
[20]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):1297-1307.
[21]黄敏.茶叶或茶青中有机磷和氨基甲酸酯类农药残留快速检测方法[J].福建分析测试,2018,27(3):1-5.
[22]王姣.QuEChERS-气相色谱-串联质谱法测定茶叶中的多种拟除虫菊酯农药[J].现代食品,2018(15):121-125.
[2]常巧英.茶叶农药多残留检测技术研究与应用[D].秦皇岛:燕山大学,2017.
[3]林建原,吴晓杰.气相色谱-质谱法(GC-MS)测定果蔬中有机磷农药残留量[J].中国食品学报,2012,12(3):160-166.
[4]苏建锋,钟茂生,陈晶.气相色谱-质谱法与气相色谱法测定测定茶叶及茶叶加工品中295种农药多残留[J].分析测试学报,2015,34(6):625-638.
[5]荣杰峰,韦航,黄伙水.羟基化多壁碳纳米管分散固相萃取/气相色谱-质谱测定茶叶中有机氯农药和拟除虫菊酯类农药残留[J].色谱,2016,35(1):8-15.
[6]董蔚,郭凯,李贺贺,等.Qu ECh ERS-GC-MS联用法检测大麦中14种邻苯二甲酸酯类塑化剂及基质效应的影响[J].食品科学,2016,37(24):156-163.
[7]XIE Q,LIU S,FAN Y,et al.Development of a dispersive liquid-liquid microextraction method for the determination of a-tocoplierol in pigmented wheat by high-performance liquid chromatography[J].Food Anal Meth,2014,7(1):21-30.
[8]李志,冯佳佳,徐俐.薏苡仁中三萜化合物的提取工艺研究[J].食品工业,2016,37(8):28-32.
[9]许秀莹,施海燕,王鸣华.气相色谱-质谱联用测定大米中6种烟碱类农药残留[J].质谱学报,2012,33(2):99-103.
[10]董金斌,王金花,卢晓宇,等.气相色谱-质谱法测定茶叶中42种残留农药[J].北京化工大学学报(自然科学版),2007(5):472-476.
[11]常淼,王崇臣,张建中,等.气相色谱测定水中19种有机氯农药[J].环境化学,2018,37(5):1165-1168.
[12]邓敏军,罗艳,邓超冰.固相萃取-气相色谱-质谱法测定水中的19种多氯联苯[J].光谱实验室,2012,29(2):947-950.
[13]赵琼晖,靳保辉,谢丽琪,等.气相色谱-质谱法测定茶叶中的25种有机氯农药残留[J].色谱,2006,32(6):629-632.
[14]曹艳平,杨路平,邵立君.气相色谱-质谱法测定茶叶中23种农药残留量[J].理化检验(化学分册),2015,51(5):647-650.
[15]曹艳平,姜大峰,李凤华,等.气相色谱-三重四极杆质谱同位素内标法测定鱼样中20种多氯联苯[J].色谱,2018,36(7):685-692.
[16]刘家曾,宋宁慧,王艺璇,等.基质固相分散-气相色谱/质谱联用技术测定茶叶中8种农药残留[J].分析科学学报,2018,34(3):337-341.
[17]刘慧,徐怡,游燕,等.气相色谱-质谱联用法测定茶叶中17种农药残留[J].广州化工,2017,45(18):87-89.
[18]李玮,贾彦博,林伟杰,等.分散固相萃取净化-气相色谱-质谱联用法测定茶叶中7种杀螨杀虫类农药残留[J].食品安全质量检测学报,2017,8(9):3485-3490.
[19]高艺羡,陈萍虹,聂丹丹,等.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):531-540.
[20]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):1297-1307.
[21]黄敏.茶叶或茶青中有机磷和氨基甲酸酯类农药残留快速检测方法[J].福建分析测试,2018,27(3):1-5.
[22]王姣.QuEChERS-气相色谱-串联质谱法测定茶叶中的多种拟除虫菊酯农药[J].现代食品,2018(15):121-125.