气相色谱-质谱联用测定奶牛血清中的β-羟丁酸

Determination of β-hydroxybutyrate in cow serum by gas chromatography-mass spectrometry (GC-MS)

为了建立测定奶牛血清中代谢产物β-羟丁酸含量的气相色谱-质谱联用方法,为奶牛酮病的早期诊断提供新途径。将奶牛血清样品用甲醇除蛋白,上清液经氮气吹干,残渣进行硅烷化衍生后,用GC-MS仪全扫描方式进行检测。结果测定血清中β-羟丁酸的线性范围为0.05 mmol/L^8 mmol/L,相关系数R=0.9995,检测限为0.03 mmol/L,定量限为0.05mmol/L,相对标准偏差RSD=5.79%,样品加标回收率为95.10%~99.91%。表明该方法能简便、快速、有效地分离并定量检测血清中的β-羟丁酸,可以作为奶牛酮病的早期诊断依据。

To establish the method of gas chromatography-mass spectrometry for measuring β-hydroxybutyrate in cow serum and provide a new way to diagnose dairy ketosis. Methanol was used for precipitating the proteins and supernate was dried by nitrogen. The concentrate was analyzed by gas chromatography-mass spectrometry after derivatization with slilylreagents. Linear relation of 13- hydroxybntyrate detected in cow serum ranged from 0.05mmol/L to 8mmol/L. The correlation coefficient was 0. 9995. The detection limit was 0. O03mmol/L and the limit of quantitation was 0.05mmol/L. Relative standard deviation was 5.79% and the adding standard recovery was 95.10% to 99.91%. The method can separate and detect 13-hydroxybutyrate in dairy serum simply, rapidly and effectively, and it is suitable for early diagnosis of dairy ketosis.