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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。
Objective To establish a method for the determination of phthalate esters in laboratory water samples by gas chromatography-mass spectrometry. Methods Take 20 ml of water sample into a 25.0 ml colorimetric tube and add 0.1 ml of 10.0 mg / L D4-DEHP internal standard solution. Mix well and purify the water sample with silica gel column (silica gel column, Methyl chloride, 5.0 ml of acetonitrile and 5.0 ml of water to activate the column) eluting the silica gel column with acetonitrile and collecting the eluate. The eluent was blown to near-dryness (50.0 ° C water bath) with nitrogen and finally to n-hexane Gas chromatography - mass spectrometry for testing, internal standard method. Results Under the experimental conditions, the chromatographic separation effects, the correlation of linear equations and the method precision of 16 kinds of phthalates were good and satisfied the experimental requirements. The correlation coefficients (r) ranged from 0.998 9 to 0.999 8. The detection limits ranged from 0.03 mg / L to 0.10 mg / L. The recoveries were 81.8% -104.0% with relative standard deviations (RSDs) of 3.1% -10.1% . Conclusion The method is convenient, rapid and sensitive. It is suitable for the determination of phthalate esters in water and at the same time is of guiding significance for the determination of phthalate esters in laboratory.