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目的利用高压液相色谱法测定东北林蛙输卵管(林蛙油)、中华绒螯蟹卵(蟹黄)以及鲫鱼卵(籽)中雌二醇的含量。方法色谱柱为Agilent Zorbax SB-C18柱(4.6 mm×250 mm,5μm),流动相为乙腈-水(63:37),检测波长280 nm,流速1.0 mL/min,柱温30℃,进样量为10μL。结果在0.3～10μg/mL浓度范围内,高压液相色谱图峰面积与雌二醇浓度线性关系良好,其回归方程为Y=4203.8X-661.95,相关系数R=0.9991。林蛙油、中华绒螯蟹卵和鲫鱼卵中雌二醇的含量分别为3.00、0.42、0.54μg/g。结论超声波法可以有效提取样品中的雌二醇,通过优化所建立的方法对其具有良好的线性关系和回收率,高压液相色谱峰型美观、分离效果好。
Objective To determine the content of estradiol in oviduct (Rana chensinensis), Eriocheir sinensis eggs (Crab roe) and crucian carp (seeds) by using high pressure liquid chromatography. Methods The column was Agilent Zorbax SB-C18 column (4.6 mm × 250 mm, 5 μm) with a mobile phase of acetonitrile-water (63:37) at a detection wavelength of 280 nm and a flow rate of 1.0 mL / The amount of 10μL. Results The peak area of high pressure liquid chromatogram was linear with the concentration of estradiol in the concentration range of 0.3 ~ 10μg / mL. The regression equation was Y = 4203.8X-661.95, and the correlation coefficient R was 0.9991. The contents of estradiol in eggs of Rana chensinensis, Eriocheir sinensis and crucian carp were 3.00,0.42,0.54μg / g respectively. Conclusion The ultrasonic method can effectively extract the estradiol in the sample. The optimized method has good linear relationship and recovery, and the HPLC method has good peak-to-peak separation effect.