S/D灭活猪血浆中磷酸三丁酯含量测定

Determination of the tributyl phosphate in S/D inactivated pig plasma by gas chromatography

建立气相色谱法测定S/D灭活猪血浆中磷酸三丁酯的含量测定方法,并进行方法学验证。该方法以正己烷为萃取剂,采用了聚乙二醇毛细管柱AgilentDB-WAX(30m×0.53mm×1μm)、氢火焰离子化检测器(FID)进行检测。方法学验证结果显示,该方法专属性良好,线性范围为0.0341~0.1024mg/ml;中间精密度所得相对标准偏差RSD仅为1.09%(n=12);以80%、100%、120%浓度水平测定的平均回收率分别为99.38%、95.66%、99.13%,9组准确度溶液测得回收率的总平均值为98.06%(n=9),RSD为2.72%(n=9)。该方法专属性较强,精密度、准确度、稳定性良好,可作为S/D灭活猪血浆中磷酸三丁酯的含量测定方法。

A gas chromatography method for the determination of tributyl phosphate in S/D inactivated pig plasma was established. Gas chromatography was performed using n-hexane as an extractant by a hydrogen flame ionization detector (FID) on an Agilent DB-WAX column (30 m×0.53 mm×1 mm). The results of methodological verification showed that the method had good specificity with a linearity over the range of 0.034 1-0.102 4 mg/ml. The relative standard deviation (RSD) obtained from the intermediate precision was only 1.09%(n=12). The average recovery rates from three samples at different concentrations (80%, 100%, 120%) were 99.38%, 95.66%, 99.13%, respectively. The total recovery rate was 98.06%(n=9) with RSD 2.72%(n=9). This method has good specificity, precision, accuracy and stability and can be used for the determination of tributyl phosphate in S/D inactivated pig plasma.