建立了一种同时测定大米中有机氯、有机磷、氨基甲酸酯和拟除虫菊酯等4类农药残留量的分析方法.通过比较二氯甲烷、三氯甲烷、乙腈、乙酸乙酯和不同比例的己烷-丙酮混合溶剂等8种溶剂的提取效果,选择以二氯甲烷为提取溶剂;以Florisil固相萃取小柱净化,通过以不同比例的己烷-丙酮作洗脱溶剂,发现体积比为4∶1的己烷-丙酮的洗脱效果最佳,在选定的洗脱条件下,样品的净化效果良好;用气相色谱-质谱测定,以保留时间、选择离子及其相对丰度定性,以外标法定量.以低限加标样品的3倍信噪比确定方法的检出限(LODs),以两个添加水平测定样品的回收率和相对标准偏差(RSD).该方法的检出限达到μg/kg水平;除敌敌畏、乐果、pp′-DDT等几种农药外,大多数农药的加标回收率在75% 和120% 之间,RSD均低于10.4% ,r≥0.992.该方法简便、快速、灵敏,能够满足同时测定大米中多种类残留农药的要求,可以作为大米中农药多残留的例行分析和确证分析的方法.
参考文献
| [1] | Liu Aijie,Yin Dulin.Journal of Natural Science of Hunan Normal University (刘爱洁,尹笃林.湖南师范大学自然科学学报),2001,24(1):50 |
| [2] | Long Su,Zhou Yigang,Wang Xiaochun,Xu Shaorui,Shu Kunxian,Luo Yaping.Practical Preventive Medicine (龙苏,周毅刚,王晓春,徐绍锐,舒坤贤,骆亚萍.实用预防医学),2001,8(5):341 |
| [3] | Schenck F J,Howard-King V.J Environ Sci Health,Part B,2000,35(1):1 |
| [4] | Yu Yong,Zou Tude.Jiangxi Chemical Industry (俞勇,邹图德.江西化工),2004(1):80 |
| [5] | Zhang Ying,Huang Zhiqiang,Chen Xinhuan.Chinese Journal of Chromatography (张莹,黄志强,陈新焕.色谱),2004,22(1):95 |
| [6] | Kang Qinghe,Yang Changzhi.Chinese Journal of Chromatography (康庆贺,杨长志.色谱),2003,21(4):421 |
| [7] | Saikia N,Kulshrestha G.J Chromatogr A,1999,864:351 |
| [8] | Lin Weixuan,Tian Miao,Li Jiye,Cao Dongmei.Journal of the Chinese Cereals and Oils Association (林维宣,田苗,李继业,曹冬梅.中国粮油学报),2003,18(2):79 |
| [9] | Hogendoorn E A,Ossendrijver F M,Dijkman E,Baumann R A.J Chromatogr A,1999,833:67 |
| [10] | Zhao Weixing,Gong Daoxin,Yang Renbin,Guo Zhengyuan,Zou Yazhu.Food Science (赵卫星,龚道新,杨仁斌,郭正元,邹雅竹.食品科学),2005,26(1):183 |
| [11] | Lin Weixuan,Li Jiye,Wang Mei,Tian Miao.Chinese Journal of Health Laboratory Technology (林维宣,李继业,王玫,田苗.中国卫生检验杂志),2001,11(1):31 |
| [12] | Dai Hua,Li Yongjun,Zhang Ying.Journal of Instrumental Analysis (戴华,李拥军,张莹.分析测试学报),2002,21(1):70 |
| [13] | Inoue T,Sasaki S,Uchikawa S,Hirahara Y,Shiomi Y,Tonogai Y.J Food Hygienic Soc Japan,2003,44(6):310 |
| [14] | Li Yongjun,Huang Zhiqiang,Yi Weiliang,Chinese Journal of Chromatography (李拥军,黄志强,易伟亮.色谱),2002,20(2):190 |
| [15] | Liu Yongbo,Jia Lihua,Niu Shuyan,Zhang Mingxia,Chen Tao.Chinese Journal of Analytical Chemistry (刘永波,贾立华,牛淑妍,张明霞,陈涛.分析化学),2005,33(2):290 |
| [16] | Jiménez J J,Bernal J L,del Nozal M J,Toribio L,Arias E.J Chromatogr A,2001,919:147 |
| [17] | Bernal J L,Jiménez J J,del Nozal M J,Higes M,Llorente J.J Chromatogr A,2000,882:239 |
| [18] | Burke E R,Holden A J,Shaw I C.Chemosphere,2003,50(4):529 |
| [19] | López-López T,Gil-Garcia M D,Martínez-Vidal J L,Martínez-Galera M.Anal Chim Acta,2001,447(1/2):101 |
| [20] | Liu Pengyan,Ma Yusong.Chemical Journal on Internet,2005,7(1):13 |
| [21] | Lin Weixuan.The Compilation of Residue Limits Standards for Pesticides and Veterinary Drugs in Foodstuffs in the World.Dalian:Dalian Maritime University Press (林维宣.各国食品中农药兽药残留限量规定.大连:大连海事大学出版社),2002:95 |
上一张
下一张
上一张
下一张
计量
- 下载量()
- 访问量()
文章评分
- 您的评分：
-
10%
-
20%
-
30%
-
40%
-
50%