[关键词]
[摘要]
建立了盐析辅助均相液液萃取结合高效液相色谱法测定蔬菜水果中对苯基苯酚残留的检测方法。试样经乙腈提取,用氯化钠盐析分层,以五氟苯基柱为色谱分离柱,甲醇-水为流动相梯度洗脱,二极管阵列/荧光双检测器,外标法定量。对提取溶剂、提取盐体系、净化、浓缩方法和稳定性等前处理的关键因素都进行了优化,并考察了不同色谱柱和流动相条件对分离效果的影响。结果表明,对苯基苯酚在0.05~100.00 μg/mL(二极管阵列检测器)和0.01~5.00 μg/mL(荧光检测器)范围内线性关系良好,相关系数(R2)均大于0.999,紫外和荧光条件下检出限分别为0.03 mg/kg和0.01 mg/kg,定量限分别为0.10 mg/kg和0.02 mg/kg。在3个空白添加浓度水平(LOQ、2LOQ和10LOQ),平均回收率分别为82.28%~110.7%和85.83%~109.8%,相对标准偏差(RSD)分别为2.60%~5.72%和2.66%~5.26%。该方法简便快捷、准确性和重现性较好,二极管阵列/荧光双串联检测可相互定性,特异性较好,适用于蔬菜水果中对苯基苯酚残留的测定。
[Key word]
[Abstract]
In this study, a analytical method was established to detect p-phenylphenol by High Performance Liquid Chromatography (HPLC) in the vegetables and fruits using salting-out homogeneous liquid-liquid extraction (SHLLE). The analyte was extracted with acetonitrile and separated from sample solution through salting-out phenomenon with sodium chloride. The separation was carried out on a reversed phase C18-PFP column using methanol and water as mobile phase and the analyte was detected with the diode array detector and fluorescence detector by HPLC, quantified by external standard method. The key factors of pre-treatment were optimized, such as extraction solvent, salt system, purification, concentration and stability, the separation effects of different chromatographic column and mobile phase conditions were investigated. The quantitative results of diode array detector and fluorescence detector indicated a good linearity of R2>0.999 in the linear range of 0.05~100.00 μg/mL and 0.01~5.00 μg/mL. The limit of detection (LOD) and quantitation (LOQ) of the diode array detector were 0.03 mg/kg and 0.10 mg/kg, and the spiked recoveries of the analyte at three different concentrations (LOQ、2LOQ和10LOQ) were in the range of 82.28%~110.7%, with RSDs in the range of 2.60%~5.72%. The limit of detection (LOD) and quantitation (LOQ) of the fluorescence detector were 0.01 mg/kg and 0.02 mg/kg, and the spiked recoveries of the analyte at three different concentrations (LOQ、2LOQ和10LOQ) were in the range of 85.83%~109.8%, with RSDs in the range of 2.66%~5.26%. With the advantage of simple, accurate, highly reproducible, the method could provide a good specificity for the determination of the p-phenylphenol with the diode array detector and fluorescence detector in the fruits and vegetables.
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