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目的建立固相萃取-气相色谱质谱联用法测定尿液中邻苯二甲酸单甲酯、邻苯二甲酸单乙酯、邻苯二甲酸单丁酯、邻苯二甲酸单2-乙基己酯、邻苯二甲酸单苄酯等5种邻苯二甲酸酯类代谢物的方法。方法尿液通过β-葡萄糖苷酶酶解,固相萃取小柱净化,三氟化硼乙醚甲醇溶液衍生,最后通过DB-5毛细管色谱柱(30m×0.25 mm,0.25μm),气相色谱质谱联用法测定。结果该方法在25.0~1000μg/L浓度范围内,5种邻苯二甲酸酯的浓度与峰面积的线性关系良好,相关系数为0.9989~0.9996,方法检出限为10.0~15.0μg/L;在空白样品中添加15.0、200和500μg/L三个浓度水平,平均回收率为80.2%~97.8%,相对标准偏差为4.2%~10.2%(n=6)。采用该方法对81位孕妇的尿液进行了检测,检出率为98.7%。结论固相萃取-气相色谱质谱联用法适用于尿液中5种邻苯二甲酸酯类代谢物的同时检测。
OBJECTIVE To establish a method for the determination of monomethyl phthalate, monoethyl phthalate, monobutyl phthalate, mono-2-ethylhexyl phthalate in urine by solid-phase extraction coupled with gas chromatography-mass spectrometry , Phthalic acid monobenzyl 5 kinds of phthalate metabolites and other methods. Methods Urine was purified by β-glucosidase enzymatic digestion, solid-phase extraction cartridge and derivatized with boron trifluoride ethereal methanol solution. Finally, the sample was separated on a DB-5 capillary column (30m × 0.25 mm, 0.25μm) Usage determination. Results The method showed a good linear relationship between the concentration of five phthalates and the peak area in the range of 25.0-1000 μg / L with the correlation coefficient of 0.9989 ~ 0.9996 and the detection limit of 10.0 ~ 15.0 μg / L. The three samples were added with different concentrations of 15.0, 200 and 500 μg / L. The average recoveries were 80.2% -97.8% with relative standard deviations of 4.2% -10.2% (n = 6). The urine of 81 pregnant women was detected by this method, the detection rate was 98.7%. Conclusion Solid-phase extraction-gas chromatography-mass spectrometry is suitable for the simultaneous detection of five phthalate metabolites in urine.