【摘要】 目的建立一种实验室用水中邻苯二甲酸酯类化合物的气相色谱-质谱测定方法。方法取20 ml水样于25.0 ml比色管中,加入0.1 ml 10.0 mg/L的D4-DEHP的内标溶液后充分混匀,将水样经硅胶柱净化后(硅胶柱预先用5.0 ml二氯甲烷,5.0 ml乙腈和5.0 ml水活化柱子),乙腈洗脱硅胶柱并收集洗脱液,洗脱液用氮气吹至近干(50.0℃水浴),最后以正己烷定容至1.0 ml,上气相色谱-质谱联用仪进行测试,内标法定量。结果在该实验条件下,16种邻苯二甲酸酯类化合物的色谱分离效果、线性方程相关性和方法精密度均良好,满足实验要求。其相关系数(r)为0.998 9~0.999 8,检出限为0.03 mg/L~0.10 mg/L,加标回收率为81.8%~104.0%,相对标准偏差(RSD)为3.1%~10.1%。结论该方法方便、快捷、灵敏度高,适用于水中邻苯二甲酸酯类化合物的测定,同时对测定邻苯二甲酸酯类化合物时实验室选择用水有一定的指导意义。更多还原

【Abstract】 Objective To establish a method for determination phthalate acid esters in laboratory water by GC-MS. Methods 20. 0 ml water samples were taken in 25. 0 ml colorimetric tube; the sample solution was well mixed after addition of0. 1 ml D4-DEHP( 10. 0 mg / L) internal standard solution and then the sample solution was purified by silica / PSA column( The silica gel column was activated with 5. 0 ml dichloromethane,5. 0 ml acetonitrile and 5. 0 ml water column in advance with acetonitrile eluting silica gel column and collection of elution solution. The elution solution was nearly dried with N2 flow to50 ℃ water bath and finally diluted to 1. 0 ml with hexane and determined by GC-MS coupling instrument and quantified with internal standard. Results Under the experimental conditions,the chromatographic separation of 16 kinds of phthalate esters,the linear equation and the method of linear equation correlation and precision of the method were good and can meet the requirement of the test. The correlation coefficient was among 0. 998 9-0. 999 8,and the spiking recovery rates were among 81. 8%-104. 0%,and the RSD was 3. 1%-10. 1%( n = 6). Conclusion This method is convenient,fast and sensitive. It is suitable for the determination of phthalate esters compounds in water,and it has a certain significance to select laboratory water for the determination of phthalate esters compounds.更多还原