复合小柱结合HPLC-MS/MS法快速测定果蔬及茶叶和大米中34种农药残留
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摘要
建立了一种运用HPLC-MS/MS的方法,通过自制的复合小柱净化以测定果蔬、茶叶和大米中34种农药残留的测定方法。采用电喷雾离子源,正离子多反应检测,液相色谱-质谱/质谱仪分离,基质曲线外标法定量。结果表明,34种农药在5～100 ng/mL的质量浓度范围内线性良好,经过乙腈提取,自制复合小柱[由900 mg无水硫酸钠(分析纯),150 mg十八弯基键合硅胶吸附剂(C_(18)),150 mg N-丙基乙二胺吸附剂(PSA),150 mg弗洛里硅藻土组成]净化,对于不同基质下的样品加标质量浓度在10.00 g/kg水平下回收率均在70%～110%。该方法简单快速、灵敏度高、耗时短、效率高,能满足平常对此34种农药的检测。
A method of HPLC-MS/MS was established to determine the determination of 34 pesticide residues in fruits,vegetables, tea and rice through the purification of self-made composite small column. In this method, liquid chromatography-mass spectrometry/mass spectrometer equipped with electrospray ion source,by positive ion multi-reaction detection,was applied to separate those pesticides,and quantified through the external standard of matrix curve. By the experiment result,34 kinds of pesticide in 5～100 ng/mL have good linear concentration range,by acetonitrile extraction,self-made composite column [ by 900 mg of anhydrous sodium sulfate(analysis), 150 mg of eighteen curved base bonded silica gel adsorbents(C_(18)),150 mg N-propyl ethylenediamine adsorbent(PSA),150 mg of Florida diatomite ] purification. For with respect to different substrate samples under concentration in 10.00 g/kg level,the average is all between 70 percent and 110 percent. In a word,this method is suitable for the detection of 34 residues of pesticides depended on its easier operation,higher sensitivity,quicker and higher efficiency.
A method of HPLC-MS/MS was established to determine the determination of 34 pesticide residues in fruits,vegetables, tea and rice through the purification of self-made composite small column. In this method, liquid chromatography-mass spectrometry/mass spectrometer equipped with electrospray ion source,by positive ion multi-reaction detection,was applied to separate those pesticides,and quantified through the external standard of matrix curve. By the experiment result,34 kinds of pesticide in 5～100 ng/mL have good linear concentration range,by acetonitrile extraction,self-made composite column [ by 900 mg of anhydrous sodium sulfate(analysis), 150 mg of eighteen curved base bonded silica gel adsorbents(C_(18)),150 mg N-propyl ethylenediamine adsorbent(PSA),150 mg of Florida diatomite ] purification. For with respect to different substrate samples under concentration in 10.00 g/kg level,the average is all between 70 percent and 110 percent. In a word,this method is suitable for the detection of 34 residues of pesticides depended on its easier operation,higher sensitivity,quicker and higher efficiency.
引文
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[7]黄玉宾,郭琳琳,刘峰.超高效液相色谱-串联三重四极杆质谱法快速测定蔬菜和水果中8种氨基甲酸酯类农药残留[J].河北农业科学,2018(2):96-99,108.
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[9] Jun Sun, Sunli Cong, Hanping Mao,et al. Quantitative detection of mixed pesticide residue of lettuce leaves based on hyperspectral technique[J]. Journal of Food Process Engineering, 2018, 41(2):12 654-12 660.
[10] Bozena Lozowicka,Ewa Rutkowska,Magdalena Jankowska. Influence of QuEChERS modifications on recovery and matrix effect during the multi-residue pesticide analysis in soil by GC/MS/MS and GC/ECD/NPD[J]. Environmental Science and Pollution Research International, 2017,24(8):7 124-7 138.
[11]郑亚丽,顾丽莉,师君丽,等.分子印迹固相萃取-高效液相色谱法同时检测烟叶中磺酰脲类农药残留[J].色谱,2018, 36(7):659-664
[2]李敏.无公害蔬菜常用农药简介[N].山西科技报,2004-11-01(004).
[3]毛敏明,周亮,肖有玉,等.农产品中常用农药残留快速检测方法概况[J].轻工标准与质量,2017(4):26-29.
[4]俞建忠,苍涛,戴芬,等.超高效液相色谱-串联质谱法测定浙贝母中6种农药残留[J].农药学学报,2018,20(3):370-376.
[5]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.
[6]李雪.气相色谱-串联质谱结合QuEChERS方法检测蔬菜、水果中37种农药残留[J].食品安全导刊,2018(18):70-71.
[7]黄玉宾,郭琳琳,刘峰.超高效液相色谱-串联三重四极杆质谱法快速测定蔬菜和水果中8种氨基甲酸酯类农药残留[J].河北农业科学,2018(2):96-99,108.
[8] Emad R. Attallah, Mahmoud Hamdy Abdelwahed, M. M.Abo-Aly. Development and validation of multi-residue method for determination of 412 pesticide residues in cotton fiber using GC-MS/MS and LC-MS/MS[J]. The Journal of the Textile Institute, 2018(1):46-63.
[9] Jun Sun, Sunli Cong, Hanping Mao,et al. Quantitative detection of mixed pesticide residue of lettuce leaves based on hyperspectral technique[J]. Journal of Food Process Engineering, 2018, 41(2):12 654-12 660.
[10] Bozena Lozowicka,Ewa Rutkowska,Magdalena Jankowska. Influence of QuEChERS modifications on recovery and matrix effect during the multi-residue pesticide analysis in soil by GC/MS/MS and GC/ECD/NPD[J]. Environmental Science and Pollution Research International, 2017,24(8):7 124-7 138.
[11]郑亚丽,顾丽莉,师君丽,等.分子印迹固相萃取-高效液相色谱法同时检测烟叶中磺酰脲类农药残留[J].色谱,2018, 36(7):659-664