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采用C18固相萃取和高效液相色谱法研究水中邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二丁酯(DBP)的萃取条件和测定条件,讨论不同的流动相中乙腈比例、检测波长、流速条件对DMP、DEP、DBP的定性和定量的影响,并对影响固相萃取效率的洗脱剂体积进行了试验研究,且成功应用在广东省珠江广州河段河涌水的检测中。结果显示,利用1.5m L的甲醇洗脱时,DMP、DEP、DBP的萃取回收率在82%~96%之间;在乙腈比例为80%、流速为0.6 m L/min、检测波长为228 nm的条件下,色谱峰完全分离,峰面积与DMP、DEP、DBP的浓度呈良好的线性关系(线性相关系数>0.999 5),检出限(LOD)为0.05~0.38μg/L,样品平均加标回收率在81.7%~109%之间,相对标准偏差(RSD)为2.3%~5.9%。该方法简便、快速,具有较高的测定准确度与精密度,适合于水中DMP、DEP、DBP的测定。
Extraction Conditions and Determination of Dimethyl Phthalate (DMP), Diethyl Phthalate (DEP) and Dibutyl Phthalate (DBP) in Water by C18 Solid Phase Extraction and High Performance Liquid Chromatography Conditions, the different mobile phase acetonitrile ratio, the detection wavelength, the flow rate of DMP, DEP, DBP qualitative and quantitative effects, and the impact of solid phase extraction efficiency of the eluent volume was studied and successfully applied in Guangdong Pearl River in Guangzhou River creek water testing. The results showed that the extraction recoveries of DMP, DEP and DBP were between 82% and 96% when the methanol was eluted with 1.5m L of methanol. When the ratio of acetonitrile was 80%, the flow rate was 0.6 m L / min and the detection wavelength was 228 nm, the peak area was completely linear with the concentration of DMP, DEP and DBP (linear correlation coefficient> 0.999 5), the limit of detection (LOD) was 0.05 ~ 0.38μg / L, the average The spiked recoveries ranged from 81.7% to 109%, and the relative standard deviations (RSDs) ranged from 2.3% to 5.9%. The method is simple and rapid, has high determination accuracy and precision, and is suitable for the determination of DMP, DEP and DBP in water.