土壤中邻苯二甲酸酯的固相萃取-毛细管气相色谱测定法

Determination of phthalate esters in soil by solid phase extraction and capillary gas chromatography

目的探讨土壤中7种邻苯二甲酸酯（PAEs）的固相萃取（SPE）-毛细管气相色谱（CGC）检测方法。方法样品经超声波提取,Pro Elut C18柱富集,甲醇-甲基叔丁基醚洗脱,DB-5色谱柱分离,氢火焰离子化检测器（FID）检测。结果邻苯二甲酸二甲酯（DMP）、邻苯二甲酸二乙酯（DEP）、邻苯二甲酸二异丙酯（Di Pr P）、邻苯二甲酸二丙烯酯（DAP）、邻苯二甲酸二丁酯（DBP）、邻苯二甲酸二戊酯（DPP）、邻苯二甲酸二辛酯（DNOP）线性范围为0.63~20.0 mg/L,其相关系数为0.999 8~0.999 9;检出限为0.02~0.09 mg/kg;精密度为2.6%~5.7%;加标回收率为78.8%~94.0%。结论该方法具有操作简便、提取效率高,检测限低,干扰小,能满足土壤样品中邻苯二甲酸酯分析的要求。

Objective To develop a method for the determination of seven phthalate esters （PAEs） in soil by solid phase extraction and capillary gas chromatography. Methods The soil sample was treated by ultrasonic extraction, concentrated by ProElut C18 column, eluted by methanol-methyl tea-butyl ether （MTBE）, separated by DB-5 column and detected by FID. Results The linear range for DMP, DEP, DiPrP, DAP, DBP, DPP and DNOP was 0.63-20.0 mg/L （r： 0.999 8-0.999 9）, the limits of detection were 0.02-0.09 mg/kg, RSDs were 2.6%-5.7%, the recovery rates were 78.8%-94.0%. Conclusion This method presents easy operation, higher extraction efficiency, lower detection limit, less interference, and is applicable to the determination for phthalate esters in soil.