气相色谱法测定左西孟旦原料药中6种有机溶剂残留量

Determination of 6 Residual Organic Solvents in Levosimendan Raw Material by GC

目的：建立测定左西孟旦原料药中6种有机溶剂即甲醇、乙醇、丙酮、二氯甲烷、异丙醇与二氧六环残留量的方法。方法：采用气相色谱法。Agilent HP-5毛细管柱,（5%）苯基-（95%）甲基聚硅氧烷为固定液;柱温采取程序升温;氢火焰离子化检测器温度为250℃;载气为高纯N2;进样口温度为200℃,分流比为10∶1;采用顶空进样法测定,顶空加热温度为100℃,加热时间为40min。结果：甲醇、乙醇、丙酮、二氯甲烷、异丙醇与二氧六环的检测质量浓度线性范围分别为150.1～449.5μg/ml（r=0.999 8）、250.6～751.2μg/ml（r=0.999 6）、249.8～749.9μg/ml（r=0.999 7）、29.09～89.68μg/ml（r=0.999 8）、250.2～750.9μg/ml（r=0.999 6）、18.91～57.92μg/ml（r=0.999 7）;平均回收率为99.9%～100.0%（RSD=0.88%～1.11%,n=3）;定量限分别为0.12、0.18、0.33、0.21、0.45、0.99 ng。样品中只检出异丙醇。结论：建立的方法快速简便,结果准确可靠。

OBJECTIVE：To establish the method for the determination of 6 residual organic solvents as methanol,alcohol,acetone,dichlormethane,isopropanol and dioxane in levosimendan raw material.METHODS：Gas chromatography was used.Capillary column（5%）phenyl-（95%）methylpolysiloxane was used as fixation fluid by temperature programming;and the temperature of flame ionization detector was 250 ℃,and high purity N2was used as carrier gas.Inlet temperature was set at 200 ℃ with split ratio of 10 ∶ 1.The conditions of headspace method included heating temperature of 100 ℃ and heating time of 40 min.RESULTS：The linear range of methanol,alcohol,acetone,dichlormethane,isopropanol and dioxane were 150.1-449.5 μg/ml（r=0.999 8）,250.6-751.2 μg/ml（r=0.999 6）,249.8-749.9 μg/ml（r=0.999 7）,29.09-89.68 μg/ml（r=0.999 8）,250.2-750.9 μg/ml（r=0.999 6） and 18.91-57.92 μg/ml（r=0.999 7）,respectively;average recoveries were 99.9%-100.0%（RSD=0.88%-1.11%,n=3）.The limits of quantification were 0.12,0.18,0.33,0.21,0.45 and 0.99 ng.Only the isopropanol was detected in samples.CONCLUSIONS：The established method is rapid,simple,accurate and reliable.