Sun Yan, Luo Laixin, Wang Fang, Li Jianqiang, Cao Yongsong
College of Agriculture and Biotechnology, China Agricultural University, No. 2 Yuanmingyuan West Road, Beijing, 100193, China.
Anal Bioanal Chem. 2009 Sep;395(2):465-71. doi: 10.1007/s00216-009-2962-y. Epub 2009 Jul 26.
A novel method based on solid-phase extraction was studied for the extraction of amitrole (3-amino-1,2,4-triazole), and its residue determination in apples has been developed. The samples were derivatized with 4-chloro-3,5-dinitrobenzotrifluoride (CNBF). The derivatization conditions and the influence of elution composition on the separation were investigated. In pH 9.5 H(3)BO(3)-Na(2)B(4)O(7) media, the reaction of amitrole with CNBF was complete at 60 degrees C after 30 min. The separation of derivatized amitrole was achieved at room temperature within 13 min by gradient elution mode with cetyltrimethylammonium bromide in mobile phase as ion-pair reagent. The method correlation coefficient was 0.9996, in concentrations ranging from 1.66 to 415 mg L(-1). The calculated recoveries of the proposed method were from 94.17% to 105.67%, and relative standard deviations were 1.57% to 6.44% in the application to the quantitative determination of amitrole in apples. The detection limit of amitrole was 0.10 mg L(-1) with a signal-to-noise ratio of 3.
研究了一种基于固相萃取的新型方法用于提取杀草强（3-氨基-1,2,4-三唑），并建立了其在苹果中残留量的测定方法。样品用4-氯-3,5-二硝基三氟甲苯（CNBF）进行衍生化。研究了衍生化条件以及洗脱组成对分离的影响。在pH 9.5的硼酸-硼砂介质中，杀草强与CNBF在60℃下反应30分钟后反应完全。以十六烷基三甲基溴化铵作为流动相中的离子对试剂，采用梯度洗脱模式在室温下13分钟内实现了衍生化杀草强的分离。该方法的相关系数为0.9996，浓度范围为1.66至415 mg L-1。该方法计算得到的回收率为94.17%至105.67%，应用于苹果中杀草强的定量测定时，相对标准偏差为1.57%至6.44%。杀草强的检测限为0.10 mg L-1，信噪比为3。
