高效液相色谱-串联质谱法同时测定贝类中22种农药残留
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摘要
建立了高效液相色谱-三重四极杆质谱(HPLC-MS/MS)同时测定贝类中22种农药残留的分析方法。样品经含0.1%(v/v)甲酸的乙腈提取,N-丙基乙二胺(PSA)和石墨化碳黑(GCB)净化,然后采用ACE UltraCore 2.5 SuperC18柱(100 mm×2.1 mm, 2.5μm)分离,以甲醇-0.1%(v/v)甲酸水溶液为流动相梯度洗脱,流速为0.4 mL/min,柱温为35℃,然后以电喷雾电离(ESI)源,在多反应监测(MRM)、正离子模式下,采用三重四极杆质谱检测。22种农药在各自的线性范围内线性关系良好,相关系数均大于0.997,检出限为0.1～0.3μg/kg,定量限为0.3～1.0μg/kg。在3个添加水平下,22种农药的平均回收率为65.2%～109.4%,相对标准偏差为1.3%～15.2%(n=6)。该方法操作简单,快速,准确度高,灵敏度高,可用于贝类中22种农药残留的同时检测。
A method for the simultaneous determination of 22 pesticide residues in shellfish by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) was developed. The pesticides in the samples were extracted with 0.1%(v/v) formic acid in acetonitrile, cleaned up with primary secondary amine(PSA) and graphitized carbon black(GCB), and then separated on an ACE UltraCore 2.5 SuperC18 column(100 mm×2.1 mm, 2.5 μm) by elution with a methanol-0.1%(v/v) formic acid solution at a flow rate of 0.4 mL/min. The analytes were detected by electrospray ionization in the positive ion mode and the multiple reaction monitoring mode. Good linear relationships were obtained, and the correlation coefficients(r~2) of the 22 pesticides were all higher than 0.997. The limits of detection and limits of quantification were 0.1-0.3 μg/kg and 0.3-1.0 μg/kg, respectively. The mean recoveries varied from 65.2% to 109.4% at three spiked levels, and the relative standard deviations ranged from 1.3% to 15.2%(n=6). The proposed method is simple, accurate, and sensitive, and is effective for the simultaneous determination of 22 pesticide residues detected in shellfish.
A method for the simultaneous determination of 22 pesticide residues in shellfish by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) was developed. The pesticides in the samples were extracted with 0.1%(v/v) formic acid in acetonitrile, cleaned up with primary secondary amine(PSA) and graphitized carbon black(GCB), and then separated on an ACE UltraCore 2.5 SuperC18 column(100 mm×2.1 mm, 2.5 μm) by elution with a methanol-0.1%(v/v) formic acid solution at a flow rate of 0.4 mL/min. The analytes were detected by electrospray ionization in the positive ion mode and the multiple reaction monitoring mode. Good linear relationships were obtained, and the correlation coefficients(r~2) of the 22 pesticides were all higher than 0.997. The limits of detection and limits of quantification were 0.1-0.3 μg/kg and 0.3-1.0 μg/kg, respectively. The mean recoveries varied from 65.2% to 109.4% at three spiked levels, and the relative standard deviations ranged from 1.3% to 15.2%(n=6). The proposed method is simple, accurate, and sensitive, and is effective for the simultaneous determination of 22 pesticide residues detected in shellfish.
引文
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[20] GB 2763-2016
[2] Papadakis E N,Tsaboula A,Kotopoulou A,et al.Sci Total Environ,2015,536(3):793
[3] Shen F,Xu Y J,Song T,et al.Chinese Journal of Chromatography,2018,36(10):1018 沈斐,许燕娟,宋挺,等.色谱,2018,36(10):1018
[4] Tankiewicz M,Biziuk M.Anal Bioanal Chem,2018,410(5):1533
[5] Cao F F,Fei J Y,Xu R J,et al.China Measurement & Test,2017,43(3):53 曹方方,费金岩,许人骥,等.中国测试,2017,43(3):53
[6] Zhong Z,Guo Y M,Liu Q.Journal of Anhui Agricultural Sciences,2015,43(23):119 钟志,郭远明,刘琴.安徽农业科学,2015,43(23):119
[7] Sun X M,Hu H M,Zhong Z,et al.J Sep Sci,2015,38(4):626
[8] Fu J W,Huang Z J,Chen M J,et al.Physical Testing and Chemical Analysis Part B:Chemical Analysis,2018,54(9):1015 符靖雯,黄子敬,陈孟君,等.理化检验-化学分册,2018,54(9):1015
[9] Fu L,Lu X B,Tan J,et al.J Environ Sci,2018,63(1):116
[10] Li L,Dong W F,Liu M Y,et al.China Food Additives,2017(7):188 李莉,董伟峰,刘梦遥,等.中国食品添加剂,2017(7):188
[11] Zhang H W,Liu H H,Tian X H,et al.Journal of Chinese Mass Spectrometry Society,2015,36(2):177 张华威,刘慧慧,田秀慧,等.质谱学报,2015,36(2):177
[12] Huang W,Zhang J J,Liu H,et al.Journal of Food Safety & Quality,2016,7(2):746 黄武,章晶晶,刘辉,等.食品安全质量检测学报,2016,7(2):746
[13] Cho H R,Park J S,Kim J,et al.Anal Bioanal Chem,2015,407(30):9043
[14] Lazartigues A,Wiest L,Baudot R,et al.Anal Bioanal Chem,2011,400(7):2185
[15] Wang X C,Shu B,Li S,et al.Talanta,2017,162:90
[16] Liu H H,Zhang H W,Wei X,et al.Chinese Journal of Analytical Chemistry,2018,46(3):386 刘慧慧,张华威,魏潇,等.分析化学,2018,46(3):386
[17] Wang Y J,Huang H L,Dong C Z,et al.Physical Testing and Chemical Analysis Part B:Chemical Analysis,2013,49(4):398 王玉健,黄惠玲,董存柱,等.理化检验-化学分册,2013,49(4):398
[18] Rahman M M,Abd El-Aty A M,Kim S W,et al.J Sep Sci,2017,40 (1):203
[19] Wang L Z,Huang X Y,Wang D F,et al.Chinese Journal of Chromatography,2015,33(5):501 王连珠,黄小燕,王登飞,等.色谱,2015,33(5):501
[20] GB 2763-2016