摘要
目的 :探讨用顶空气相色谱法测定那屈肝素钙中乙醇残留量的准确性。方法 :使用顶空气相色谱法,对我公司生产的3个批次那屈肝素钙中乙醇的残留量进行测定,并计算出那屈肝素钙中乙醇的线性关系、回收率和RSD。结果 :那屈肝素钙样品中残留的乙醇和正丙醇分离度良好,其中乙醇在0.125~1.5mg/m L的范围内其线性关系良好(r=0.9994),其平均加样回收率为105.3%,其RSD值为4.41%。结论 :用顶空气相色谱法测定那屈肝素钙中乙醇残留量具有操作简单、速度快和准确率高的优点。此方法值得在临床上推广使用。
objective to adopt to establish a gas chromatography determination of ethanol in the flexor heparin calcium API residue method. Methods using headspace gas chromatography, capillary chromatographic column models for DB-624, which contains (6%6%of the cyanide propyl stupid, dimethyl polysiloxane, specifications for:30 m*0.53 mu m*3.0 microns), with internal standard are propanol substrates, nitrogen as carrier gas, column temperature, temperature programmed, initial temperature 40℃, keep 4 min. In order to 3℃to 58℃per minute;Again in 20℃/min up to 160℃. Injection port temperature 150℃, FID detector temperature 250℃. Head space equilibrium temperature 80℃, balance time 20 min. Results ethanol, normal propyl alcohol degree of separation, the ethanol in the range of 0.125~1.5 mg/mL inside have good (r=0.9994), the average sample recovery rate was 105.3%, RSD was 4.41%. Conclusion the method is simple and rapid operation, high sensitivity, good accuracy, can be used as the flexor heparin calcium ethanol residue determination.
