通窍镇痛散的质量标准研究

目的 建立通窍镇痛散质量控制方法.方法 采用TLC法对制剂中的木香进行了定性鉴别；用气相色谱法对制剂中的丁香、冰片进行了定性鉴别,气相色谱柱为弹性石英毛细管柱DB-WAX （30 mm×0.25 mm,0.25 μm）,氮气为载气,FID检测器,柱温130℃,检测器温度为200℃,分流比为6∶1.用高效液相色谱法测定了制剂中胡椒碱的含量.色谱柱：Extend-C18（250 mm×4.6 mm,5μm）；流动相：乙腈-水（45∶55）；检测波长：343 nm;流速：1.0 mL· min-1.结果 胡椒碱的加样回收率平均值为97.26％,RSD为1.37％（n=6）.TLC、GC鉴别阴性无干扰.结论 试验结果表明,该方法准确、灵敏度高,重现性好.

Research on Quality Standards of Tongqiaozhentong Powder

Objective To establish a quality control method for tongqiaozhentong powder. Methods Radix Aucklandiae was identified by TLC. FlosCaryophylli, （ ±） -Borneoland （ ± ） ＋ Isoborneolwere identified by GC. A DB-WAX capillary column （30 mm × 0.25 mm, 0.25 μm） was adopted in the GC system with the column temperature at 130 ℃, nitrogen was used as the carrier gas, FID as the detector at 200 ℃, and the split ratio was 6 ： 1. The contents of Piperine in this preparation were determined by HPLC. Extend-C18 （250 mm×4.6 mm, 5 μm） column was used as the stationary phase, with a mobile phase of acetonitril-water acid solution （45 × 55）, the detection wavelength was 343 nm and the flow rate was 1.0 mL · min^- 1. Results The mean recovery of Piperine in tongqiaozhentong powder was 97.26%（RSD=1.37%） （n=6）. The negative sample didn＇t interfere the identification of TLC or GC. Conclusion The results showed that the established method is accurate, sensitive and reproducible.