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目的建立膝关节炎外敷贴剂中挥发油含量测定方法。方法采用气相色谱法测定膝关节炎外敷贴剂中挥发油的含量。色谱法分析条件为,PDI检测器;色谱柱,聚乙二醇-20M为固定相,流动相载气:高纯氮气毛细管柱;进样口温度为220℃,检测器温度为250℃。柱温采用程序升温,初始温度90℃,保持1 min,升温速度6℃/min,升至120℃,再以0.4℃/min升温至125℃,最后以10℃/min升温至230℃。流速:25 ml/min,进样量:1μl,定量方法:内标法;理论塔板≥15 000。结果挥发油含量在0.161 9~0.809 6 mg/ml范围内线性关系良好,得回归方程y=0.307 1x+0.024 6,r=0.999 6,平均回收率为100.1%,RSD为1.15%。结论本方法简便可行、结果准确可靠,重复性好,可作为膝关节炎外敷贴剂中挥发油含量测定方法。
Objective To establish a method for the determination of volatile oil in external application of knee arthroplasty. Methods Gas chromatographic method was used to determine the content of volatile oil in external application of knee arthroplasty. The chromatographic conditions were: PDI detector; column, polyethylene glycol-20M as stationary phase, mobile phase carrier gas: high purity nitrogen capillary column; inlet temperature was 220 ℃ and detector temperature was 250 ℃. The temperature of the column was increased by programmed temperature, the initial temperature was 90 ℃, maintained for 1 min, the temperature was raised to 6 ℃ / min, then increased to 120 ℃, and then heated to 125 ℃ at 0.4 ℃ / min and finally to 230 ℃ at 10 ℃ / min. Flow rate: 25 ml / min, injection volume: 1μl, quantitative method: internal standard method; theoretical plate ≥15000. Results The volatile oil content was good in the range of 0.161 9-0.809 6 mg / ml. The regression equation y = 0.307 1x + 0.024 6, r = 0.999 6, the average recovery was 100.1% and the RSD was 1.15%. Conclusion The method is simple and feasible, accurate and reliable, good repeatability, and can be used as a method for determination of volatile oil in external application of knee arthroplasty.