气相色谱法测定盐酸普拉格雷中的异丙叉丙酮和佛尔酮

Determination of Mesityl Oxide and Phorone in Prasugrel Hydrochloride by Gas Chromatography

建立了气相色谱法测定盐酸普拉格雷(1)中含警示结构不饱和酮的异丙叉丙酮(2)和佛尔酮(3)。色谱柱采用DB-624毛细管柱(30 m×0.53 mm×3.0μm),程序升温,采用直接进样法进行测定。结果显示,2、3在5~30μg/ml内线性关系良好,平均回收率(n=9)分别为101.25%、102.23%,RSD分别为0.66%、0.79%。2、3的定量限分别为2.77、2.89μg/ml,检测限分别为1.11、1.16μg/ml。建立的方法专属性强、灵敏度高、耐用性好,可用于1中2和3的测定。

A gas chromatographic method was established for determination of the structural alerts,the unsaturated ketones mesityl oxide(2)and phorone(3),in prasugrel hydrochloride(1).The DB-624 capillary column(30 m×0.53 mm×3.0μm)was used with temperature programming,and the direct injection method was used for the determination.The results showed that it was linear for 2 and 3 in the range of 5-30μg/ml,the average recoveries(n=9)of 2 and 3 were 101.25%and 102.23%,with the RSDs of 0.66%and 0.79%,respectively.The limits of quantification of 2 and 3 were respectively 2.77 and 2.89μg/ml,and the limits of detection were respectively 1.11 and 1.16μg/ml.The established method has strong specificity,high sensitivity and good durability,which can be used for the determination of 2 and 3 in 1.