分散固相萃取法直接萃取水样中16种邻苯二甲酸酯

Direct Extraction of 16 Phthalate Acid Esters in Water Samples by Dispersive Solid-Phase Extraction

将固相萃取柱填料HC—C18作为萃取剂直接分散于水样中，经振荡萃取后用固相萃取空柱过滤回收萃取剂，经过洗脱、浓缩后，用气相色谱／质谱联用仪对水样中的16种邻苯二甲酸酯进行分析测定。实验对萃取剂的种类和用量、水样pH、萃取时间及洗脱剂等影响因素进行了选择和优化。当萃取剂为0．3gHC—C18、水样pH为2、振荡萃取10min、洗脱剂为6mL二氯甲烷一乙酸乙酯（体积比1：1）时，16种邻苯二甲酸酯具有较好的回收率，在0．02～40μg／L范围内线性良好，相关系数在0．9861～0．9999之间，检出限为5～400ng／L；实际水样测定的相对标准偏差在1．9％～11．6％（n=6）之间，加标回收率为81．5％～109．2％。该方法操作简单省时，能够同时满足水中16种邻苯二甲酸酯的分析测定。

HC-C18 ,traditionally used filler of SPE column,was dispersed in the water as the extractant. Sixteen phthalate acid esters （PAEs） in water samples were analyzed by gas chromatography-mass spectrometry after extraction, elution and concentration. The influence factors such as extractant, pH, extraction time and eluant were optimized. The optimal conditions turn out to be.extractant of 0.3 g HC- C18 ; pH of 2 ~ extraction time of 10 min ~ eluant of 6 mL dichloromethane and ethyl acetate（1＂ 1 ,V/V）. The recoveries were highest for almost 16 PAEs under the optimal conditions. For 16 PAEs, the linear calibration curves were in the range of 0.02-40 /~g/L and the correlation coefficients（R2） were between 0. 9861 and 0. 9999, the limits of detection were 5-400 ng/L, the relative standard deviations （RSDs, n = 6） of real water samples were 1.9%-11.6% and the recoveries were 81.5%-109.2o//oo. It was suitable for determination of PAEs in surface water.