高效液相色谱-串联质谱法测定血清中的雌激素

Determination of estrogen in serum by high performance liquid chromatography tandem mass spectrometry

目的建立同位素内标-高效液相色谱-串联质谱方法测定人血清中3种雌激素的含量。方法采用高效液相色谱-串联质谱仪,色谱柱为Phenomenex Gemini■3μm C_(18)110A(50 mm×3 mm),柱温40℃。流动相为0.1%氨水溶液:甲醇,流速为0.6 ml/min。在电喷雾负离子模式下,采用多反应监测模式对血清中雌激素含量进行定量。结果3种雌激素在相应的浓度范围内相关系数r均大于0.997,加标回收率为91.76%~105.90%,精密度为0.25%~3.04%,无携带污染。结论该方法准确、可靠、灵敏度好、专属性强,适用于血清中雌激素的检测。

Objective To establish a method for the determination of three estrogens in human serum by isotope internal standard-high-performance liquid chromatography-tandem mass spectrometry.Methods A high-performance liquid chromatography tandem mass spectrometer was used.The chromatographic column is Phenomenex Gemini■3μm C_(18)110A(50 mm×3 mm),and the column temperature was 40℃.The mobile phase was 0.1%ammonia water:methanol,with a flow rate of 0.6 ml/min.Under the mode of electric spray anion,the content of estrogen in serum was quantified by multi reaction detection mode.Results The correlation coefficients(r)of the three estrogens were all greater than 0.997 in the corresponding concentration range.The spiked recoveries was 91.76%-105.90%,the precision was 0.25%-3.04%,and no carryover contamination.Conclusion The method is accurate,reliable,sensitive,and highly specific,and can be used for the detection of estrogen in serum.