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建立了一种加速溶剂萃取-凝胶色谱净化-气相色谱/质谱联用法快速测定水产加工品中胆固醇氧化物含量的分析方法。采用此分析方法,测定了胆甾烯酮、7β-羟基胆固醇、5β,6β-环氧化胆固醇、5α,6α-环氧化胆固醇、20α-羟基胆固醇、3β,5α,6β-胆甾烷三醇、6-酮基胆固醇、7-酮基胆固醇等8种化合物,优化了加速溶剂萃取仪、凝胶净化色谱仪、气相色谱/质谱联用仪的条件,在10~1000 ng/m L范围内,线性相关系数可达0.9995以上;重现性良好,其相对标准偏差小于7%;回收率可达76%~103%;其灵敏度高,方法检测限低:8种胆固醇氧化物为0.1μg/kg以下,适用于水产加工品中胆固醇氧化物的检测工作。
An analytical method was established for the rapid determination of cholesterol oxide in aquatic products by accelerated solvent extraction-gel chromatography purification-gas chromatography / mass spectrometry. Cholesterone, 7β-hydroxycholesterol, 5β, 6β-epoxidized cholesterol, 5α, 6α-epoxidized cholesterol, 20α-hydroxycholesterol, 3β, 5α, 6β- Alcohol, 6-keto-cholesterol and 7-keto-cholesterol, the conditions of accelerated solvent extraction, gel purification and gas chromatography / mass spectrometry were optimized. , The linear correlation coefficient can reach above 0.9995; the reproducibility is good, the relative standard deviation is less than 7%; the recovery rate is up to 76% ~ 103%; the sensitivity is high and the detection limit of the method is low: 0.1 μg of 8 kinds of cholesterol oxide / kg or less, suitable for the detection of cholesterol oxide in aquatic products.