基于气相色谱-飞行时间质谱的烟叶农残定性筛查和定量分析
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摘要
建立了一种基于气相色谱-飞行时间质谱的烟叶农残定性筛查和定量分析方法。方法利用气相色谱-飞行时间质谱灵敏度高、扫描速度快等特点,在25 min的仪器分析时间内实现了烟叶农残定性筛查和定量分析数据的同时采集。通过建立基于保留时间和特征离子的定性筛查表,实现了烟叶中1300种农药残留的筛查,通过基质添加标准曲线的绘制,实现了84种烟叶中高概率检出农药的定量分析。其中,84种农药的基质添加标准曲线的线性相关系数(r2)在0. 9914～0. 9999之间,回收率在72. 1%～109. 3%之间,重复性在2. 1%～13%之间,定量限在0. 9～14. 4μg/kg之间。
A gas chromatography-time-of-flight mass spectrometry( GC-TOFMS) based method was established for the screening and quantitation of pesticide residues in tobacco leaves. The GC-TOFMS raw data of the established method were acquired in 25 min because of the high sensitivity and fast screening of the TOFMS. The screening table based on retention time and characteristic ions was constructed and the existence of 1300 of pesticides in each tobacco sample was judged. Quantitation of84 commonly used tobacco pesticides was also performed based on matrix added standard curves.Correlation coefficients( r2) of the standard curves ranged from 0. 9914 to 0. 9999,with recoveries from 72. 1% to 109. 3%,repeatabilities from 2. 1% to 13%,and limits of quantitation from 0. 9 μg/kg to 14. 4 μg/kg.
A gas chromatography-time-of-flight mass spectrometry( GC-TOFMS) based method was established for the screening and quantitation of pesticide residues in tobacco leaves. The GC-TOFMS raw data of the established method were acquired in 25 min because of the high sensitivity and fast screening of the TOFMS. The screening table based on retention time and characteristic ions was constructed and the existence of 1300 of pesticides in each tobacco sample was judged. Quantitation of84 commonly used tobacco pesticides was also performed based on matrix added standard curves.Correlation coefficients( r2) of the standard curves ranged from 0. 9914 to 0. 9999,with recoveries from 72. 1% to 109. 3%,repeatabilities from 2. 1% to 13%,and limits of quantitation from 0. 9 μg/kg to 14. 4 μg/kg.
引文
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[3] Lou X H,Gao C C,Zhu W J,Zhang X Y,Shi X Y. Chin. J. Tob. Sci.,2012,33(5):83楼小华,高川川,朱文静,张晓瑜,史训瑶.中国烟草科学,2012,33(5):83
[4] Lin S,Luo L,Yao B B,Guo J J,Zhu H L,Ding Y. Chin. J. Anal. Lab.,2017,36(1):114林森,罗亮,姚帮本,郭佳佳,祝红蕾,丁燕.分析试验室,2017,36(1):114
[5] Cao J M,Qiu J,Yu W S,Fang S,Lu S J,Lin Y N,Wang L L,Guo C F. Chin. J. Anal. Lab.,2012,31(11):24曹建敏,邱军,于卫松,方松,鲁世军,林樱楠,王丽丽,郭承芳.分析试验室,2012,31(11):24
[6] Wang J G,Wan L K,Wei Y X,Liu X F,Guo H,Yang Y Z,Li B. Chin. J. Anal. Lab.,2017,36(2):220王建国,万丽葵,魏玉霞,刘晓峰,郭虹,杨玉竹,李博.分析试验室,2017,36(2):220
[7] Si X X,Zhu R Z,Liu Z H,Ma X Y,Zhu L,Zhang F M,Liu C B. J. Instr. Anal.,,2016,35(5):532司晓喜,朱瑞芝,刘志华,马雪英,朱丽,张凤梅,刘春波,陆舍铭.分析测试学报,2016,35(5):532
[8] Si X X,Lu S M,Liu Z H,Zhu L,Liu C B,Zhang F M,He P,Zhu R Z. Chinese. J. Chromatogr.,2016,34(3):340司晓喜,陆舍铭,刘志华,朱丽,刘春波,张凤梅,何沛,朱瑞芝.色谱,2016,34(3):340
[9] Si X X,Zhu R Z,Zhang F M,Lu S M,Zhu L,Leng S X,Xie J,Liu C B,Liu Z H. Chinese. J. Chromatogr.,2016,34(6):608司晓喜,朱瑞芝,张凤梅,陆舍铭,朱丽,冷思漩,谢姣,刘春波,刘志华.色谱,2016,34(6):608
[10] Ai D,Hu B,Pan L N,Chen L,Liu. H M. Tob Sci Technol,2014,(4):79艾丹,胡斌,潘立宁,陈黎,刘惠民.烟草科技,2014,(4):79
[11] Mondello L. http://www. sisweb. com/software/wiley-pesticideswithri. htm#1,2016(accessed December 25. 2017)
[12] Q/T 47. 1-2014,Tobacco and tobacco products-Determination of multi-pesticide residues-Part 1:Gas chromatographytandem mass spectrometry method Q/T 47. 1-2014,烟草及烟草制品多种农药残留量的测定第1部分:气相色谱-串联质谱联用法
[13] Guedes J A,Silva R O,Lima C G,Milhome M A,do Nascimento R F. Food Chem.,2016,199:380
[14] Pano-Farias N S,Ceballos-Magana S G,Muniz-Valencia R,Jurado J M,Alcazar A,Aguayo-Villarreal I A. J. Food Drug Anal.,2017,25(3):501
[15] Vandendool H,Kratz P D. J. Chromatogr.,1963,11(4):463
[16] Davies A N. Spectrosc. Eur.,1998,10(3):24