用HPLC—ESI-TOFMS建立了快速灵敏检测尿中雌二醇的方法,尿样中雌二醇经盐酸水解后用OASISHLB小柱萃取.色谱柱为XTerraMS C18反相分离柱(3.5μm,2.1mm×100mm),流动相为水和乙腈,梯度洗脱,流速为0.2mL/min,紫外检测波长为280nm,外标法定量.质谱采用负离子电离模式.线性方程:y=1.79×10^5x+2.59×10^4,线性范围:0.0328—32.8mg/L,线性相关系数R^2=0.9979,最小检出浓度0.00328mg/L,萃取回收率101.83%.应用本方法对10例正常人尿样进行测定,结果满意.相比较其它检测尿中雌二醇的方法来说,此法比较简单、快速、准确,为临床的诊断提供有价值的指标.
By using HPLC-ESI-TOF MS, we established a convenient and rapid method for detecting estradiol in human urine. The target compounds in urine were firstly hydrolyzed in HCl medium and extracted by OASIS HLB columns. The separation was carried out on a XTerra MS C18 (3.5 μm, 2.1 mm × 100 mm) RP column at 35 ℃ with a linear gradient elution of water(A) -acetonitrile(B). The flow-rate of 0.2 mL/min and UV detection at 280 nm were used in this study. The Mass was in negative mode. The limit of detection and the linear range of estradiol were 0.003 28mg/L and 0. 032 8 32.8 mg/L respectively, with extraction recovery rate of 101.83 % . This method has been applied to the determination of estriol in 10 human urine samples with satisfactory results.