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目的研究固相萃取-高效液相色谱法同时测定人体卵泡中4种邻苯二甲酸酯代谢物的方法。方法采用固相萃取对卵泡样品进行前处理,固相萃取柱采用HLB小柱,选用3 ml乙腈、3 ml乙酸乙酯和3 ml乙醚作为洗脱剂对小柱进行洗脱。选择C6H5色谱柱,以乙腈-水体系为流动相,以高效液相色谱方法测定邻苯二甲酸酯代谢物。结果 4种邻苯二甲酸酯代谢物的线性范围为10~4 000μg/L,检出限为4.69~7.63μg/L,相对标准偏差为2.69%~11.38%,回收率范围为81.89%~90.29%。结论该方法准确、灵敏,精密度好,适于卵泡液中邻苯二甲酸酯的测定。
Objective To study a method for the simultaneous determination of 4 phthalate metabolites in human follicles by solid-phase extraction and high performance liquid chromatography. Methods Follicular samples were pretreated by solid phase extraction. The solid phase extraction column was eluted with HLB cartridge using 3 ml of acetonitrile, 3 ml of ethyl acetate and 3 ml of diethyl ether as eluant. The C6H5 column was used to determine the phthalate metabolites by acetonitrile-water system. Results The linear range of the four phthalate metabolites was 10-4000μg / L with the detection limits of 4.69-7.63μg / L and the relative standard deviations of 2.69% ~ 11.38%. The recoveries ranged from 81.89% 90.29%. Conclusion The method is accurate, sensitive and accurate. It is suitable for the determination of phthalates in follicular fluid.