Zhao Tao, Wang Qingqing, Li Jie, Qiao Xuguang, Xu Zhixiang
College of Food Science and Engineering, Shandong Agricultural University, Taian, 271018, China.
J Sci Food Agric. 2014 Aug;94(10):1974-80. doi: 10.1002/jsfa.6511. Epub 2014 Jan 2.
Organophosphorus pesticides have been widely used in agricultural production. However, the wide use of organophosphate also results in pesticide residues on the plant, which are harmful to human health because of their potential mutagenic and carcinogenic properties. Therefore, it is vital to develop a sensitive and effective analysis method to control pesticide residues.
In this study, a novel molecularly imprinted capillary monolithic column was prepared using trichlorfon as the template molecule by combining non-hydrolytic sol-gel process with a molecular imprinting technique. The resulting material was characterized by scanning electron microscopy and Fourier transform infrared. Under capillary electrochromatography, the effects of voltage, pH, ACN content and concentration of buffer solution on the electro-osmotic flow (EOF) of imprinted capillary monolithic column were evaluated in detail. Using this prepared material as stationary phase for capillary electrochromatography, a novel method of molecularly imprinted capillary electrochromatography (MICEC) for the detection of trace trichlorfon residues in vegetables was developed. Under optimal conditions, appreciable sensitivity was achieved with a LOD (S/N = 3) of 92.5 µg kg(-1) and method quantitation limit (MQL) of 305.3 µg kg(-1), respectively. The linear ranges of the calibration graph were 0.1 µg L(-1) to 10 mg L(-1). The peak area precision (RSD) for five replicate extractions of 0.01 mg L(-1) trichlorfon standard aqueous solution was 4.5%. To evaluate the accuracy of this method, the blank cucumber and cauliflower samples spiked with trichlorfon were extracted and analyzed by this method with good recoveries, ranging from 80.2% to 95.8%. Moreover, this method was successfully applied to the quantitative detection of the trichlorfon residues in leek samples.
With good properties of high sensitivity and simple pre-treatment, this MICEC method could provide a new tool for the rapid determination of trace trichlorfon residue in complex food samples.
有机磷农药已广泛应用于农业生产。然而,有机磷农药的广泛使用也导致植物上有农药残留,由于其潜在的诱变和致癌特性,这些残留对人体健康有害。因此,开发一种灵敏有效的分析方法来控制农药残留至关重要。
在本研究中,通过非水解溶胶 - 凝胶法与分子印迹技术相结合,以敌百虫为模板分子制备了一种新型分子印迹毛细管整体柱。所得材料通过扫描电子显微镜和傅里叶变换红外光谱进行表征。在毛细管电色谱条件下,详细评估了电压、pH值、乙腈含量和缓冲溶液浓度对印迹毛细管整体柱电渗流(EOF)的影响。以制备的这种材料作为毛细管电色谱的固定相,开发了一种用于检测蔬菜中痕量敌百虫残留的新型分子印迹毛细管电色谱(MICEC)方法。在最佳条件下,实现了可观的灵敏度,检测限(S/N = 3)为92.5 μg kg⁻¹,方法定量限(MQL)为305.3 μg kg⁻¹。校准曲线的线性范围为0.1 μg L⁻¹至10 mg L⁻¹。0.01 mg L⁻¹敌百虫标准水溶液五次重复萃取的峰面积精密度(RSD)为4.5%。为评估该方法的准确性,对添加了敌百虫的空白黄瓜和花椰菜样品进行萃取并通过该方法分析,回收率良好,范围为80.2%至95.8%。此外,该方法成功应用于韭菜样品中敌百虫残留的定量检测。
这种MICEC方法具有高灵敏度和简单预处理的良好特性,可为快速测定复杂食品样品中痕量敌百虫残留提供一种新工具。