顶空气相色谱法测定丹参素冰片酯脂肪乳中溶剂残留量

Determination of residual solvents in Danshensu Borneol Ester Fat Emulsion Injections by headspace capillary GC

目的建立顶空毛细管气相色谱法测定丹参素冰片酯脂肪乳注射液的溶剂残留量。方法采用顶空毛细管气相色谱法。色谱柱为DB-WAX(30m×0.25mm,0.25μm)毛细管色谱柱;柱温40℃;载气为氮气,柱流速为2.0mL.min-1;采用分流进样,分流比为1∶1;进样口温度200℃,FID检测器温度为230℃。结果甲醇、乙醇、乙醚、丙酮、四氢呋喃、乙酸乙酯的线性范围分别为:6～238μg·mL-1(r=0.998 9),10～395μg·mL-1(r=0.997 9),10～400μg·mL-1(r=0.998 0),10～394μg·mL-1(r=0.998 6),2～53μg·mL-1(r=0.997 4)和10～414μg·mL-1(r=0.997 1);平均回收率分别为96.6%,96.8%,96.2%,92.1%,92.9%和93.2%,其RSD分别为1.0%,0.2%,1.1%,1.0%,0.8%和1.4%。结论该法操作简便可靠,适用于丹参素冰片酯脂肪乳注射液中有机溶剂残留的检测。

Objective To establish a handspace capillary GC method for the determination of residual solvents in Danshensu Borneol Ester Fat Emulsion Injections. Method A headspace capillary GC was established, and the experimental conditions were as follows： A DB-WAX capillary column （30 m×0.25 mm,0.25 μm） was used at 40 ℃. N2 was used as the carrier gas at a column flow rate of 2.0 mL·min^-1 ,the split rate was 1： 1. The injector temperature was 200 ℃. FID detector was used at 230℃. Results The linear ranges of methanol, ethanol, ether, acetone, tetrahydrofuran, and ethyl acetate were 6-238 μg·mL^-1 （r= 0. 998 9 ）, 10-395μg·mL^-1 （r=0. 997 9） ,10-400μg·mL^-1（r=0. 998 0） ,10-394 μg·mL^-1（r=0. 998 6） ,2-53 μg·mL^-1 （r=0. 997 4） and 10-414μg·mL^-1 （r=0. 997 1） ,respectively. The average recoveries were 96. 6%,96.8%,96.2%,92. 1%,92.9% and 93.2% ,and the RSD were 1.0 % ,0.2 %, 1.1%, 1.0 %, 0. 8 % and 1.4 %, respectively. Conclusion The method is accurate and reliable. It can be applied for the detection of residual solvents in Danshensu Borneol Ester Fat Emulsion Injections.