建立了分散液液微萃取( DLLME)与气相色谱-质谱法( GC-MS)联用快速检测蜂蜜中六六六( BHC)和滴滴涕( DDT)类农药残留的分析方法。使用三氯甲烷为萃取剂,通过涡旋、离心使分析物富集到微量三氯甲烷中,采用气相色谱-质谱进行分析。实验对影响 DLLME萃取效率的因素,如萃取剂种类和体积、分散剂种类和体积、萃取时间等进行了考察,同时对方法的基质效应和性能进行了评估。结果显示:由于基质效应,8种六六六和滴滴涕类农药都出现信号增强现象。8种六六六和滴滴涕类农药在2~500μg/L范围内线性关系良好,相关系数( r2)为0.991~0.998,方法富集倍数为74~96;当试样的加标水平为20、50和100μg/kg时,8种六六六和滴滴涕类农药的回收率为61.0%~100.1%,相对标准偏差( RSD,n=5)为2.2%~19.5%。8种六六六和滴滴涕类农药的最低检测浓度均为20μg/kg,最小检出量皆为1.0 ng。该方法简单、快速、高效,适用于蜂蜜中六六六和滴滴涕类农药的残留检测。
A gas chromatography-mass spectrometry( GC-MS)method for the determination of hexachlorocyclohexane(BHC)and dichlorodiphenyltrichloroethane(DDT)residues in honey was developed using dispersive liquid-liquid microextraction( DLLME ) as sample preparation method. The samples were extracted with chloroform,and concentrated into chloroform by vortex and centrifuging. The analytes were analyzed by GC-MS. The factors affecting the extrac-tion efficiency were investigated,such as the type and volume of extraction and dispersive sol-vent,extraction time,etc. The matrix effects and method performance were evaluated at the same time. The results indicated that all the eight BHC and DDT pesticides displayed the enhancement of signals due to the matrix effects. The calibration curves were linear in the range of 2-500 μg/L and the correlation coefficients were 0. 991-0. 998 for the eight BHC and DDT pesticides. The enrichment factors( EF)were 74-96 for the eight pesticides. The recover-ies of the eight BHC and DDT pesticides at three spiked levels of 20,50 and 100 μg/kg were 61. 0%-100. 1%,while the RSDs were 2. 2%-19. 5%. The limits of quantification for the eight pesticides were 20 μg/kg,and the limits of detection were 1. 0 ng. The developed method is easy,quick and with high performance. It is applicable for the determination of BHC and DDT residues in honey.
参考文献
[1] | Song S L,Rao Z. Chinese Journal of Pesticide Science(宋淑玲,饶竹. 农药学学报),2011,13(5):439,2011. |
[2] | Li Q Z,Zhu M,Ren D X,et al. Journal of Sichuan of Tradi-tional Chinese Medicine(李琦智,朱敏,任德鑫,等. 四川中医),2004,22(1):30,2004. |
[3] | Gu X Z,Li X D,Mao S J,et al. Chinese Journal of Experi-mental Traditional Medical Formulae(顾雪竹,李先端,毛淑杰,等. 中国实验方剂学杂志),2007(6):70,2007. |
[4] | Wang X X,Cheng X J,Xu W S,et al. Guangxi Agricultural Science(王新雄,成秀娟,徐伟松,等. 广西农业科学), 2008,39(5):700,2008. |
[5] | Xia G H,Shen W J,Yu K Y,et al. Chinese Journal of Chro-matography(夏广辉,沈伟健,余可垚,等. 色谱),2014,32 (7):741,2014. |
[6] | Zacharis C K,Rotsias I,Zachariadis P G,et al. Food Chem, 2012,134:1665,2012. |
[7] | Lin Z G,Jin Z,Ma Y,et al. Chinese Journal of Analysis Laboratory(林竹光,金珍,马玉,等. 分析实验室),2006, 25(6):12,2006. |
[8] | Fang Y L,Wang S E,Shao L H,et al. Journal of Environ-ment and Health(方英立,王淑娥,邵丽华,等. 环境与健康杂志),2007,24(10):807,2007. |
[9] | Kujawski M W,Pinteaux E,Namiesnik J. Eur Food Res Technol,2012,234:223,2012. |
[10] | Zhang X L,Jiao B N. Food Science(张雪莲,焦必宁. 食品科学),2012,33(9):307,2012. |
[11] | Jovanov P,Guzsvány V,Franko M,et al. Talanta,2013, 111:125,2013. |
[12] | Zhang J H,Gao H X,Peng B,et al. J Chromatogr A,2011, 1218:66,2011. |
- 下载量()
- 访问量()
- 您的评分:
-
10%
-
20%
-
30%
-
40%
-
50%