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目的:建立大蒜油静脉注射乳剂指纹图谱及指标成分含量测定的方法。方法:采用气相色谱(GC)法测定大蒜油静脉注射乳剂指纹图谱及制剂中大蒜素含量。色谱柱为HP-5(30m×320μm×0.25μm),进样口温度为250℃,柱温为60～220℃,程序升温,载气为N2,流速为1.0mL·min-1,FID检测器,检测室温度为300℃,以四氢呋喃为内标。结果:大蒜素检测浓度在0.05～2.4mg·mL-1范围内同其与内标峰面积比呈良好线性关系(r=0.9998);平均回收率为102.5%(RSD=0.41%,n=9)。大蒜油静脉注射乳剂指纹图谱确定共有峰17个,日内相对保留时间和相对峰面积的RSD分别小于0.05%和8%,室温放置48h后相对保留时间和相对峰面积的RSD分别小于0.08%和15%,重复性试验相对保留时间和相对峰面积的RSD分别小于0.04%和8%。结论:大蒜油静脉注射乳剂指纹图谱及含量测定方法准确可靠、简便可行,能有效控制大蒜油静脉注射乳剂的质量。
Objective: To establish the method of fingerprinting and index component determination of garlic oil intravenous emulsion. Methods: The gas chromatogram (GC) method was used to determine the fingerprints of garlic oil intravenous emulsion and the content of allicin in the preparation. The column is HP-5 (30m×320μm×0.25μm), inlet temperature is 250°C, column temperature is 60～220°C, program temperature, carrier gas is N2, flow rate is 1.0mL·min-1, FID detection The temperature of the test chamber is 300°C and tetrahydrofuran is used as the internal standard. RESULTS: The detection concentration of allicin in the range of 0.05-2.4 mg·mL-1 showed a good linear relationship with its internal standard peak area ratio (r=0.9998); the average recovery was 102.5% (RSD=0.41%, n=9 ). A total of 17 common peaks were identified in the emulsion fingerprints of garlic oil intravenous injection. The RSDs of the relative retention time and relative peak area were less than 0.05% and 8%, and the RSDs of relative retention time and relative peak area were less than 0.08% and 15% after 48 hours at room temperature. %, RSDs for relative retention times and relative peak areas for reproducibility tests were less than 0.04% and 8%, respectively. Conclusion: The fingerprints and determination methods of intravenous emulsion of garlic oil are accurate, reliable, simple and feasible, and can effectively control the quality of garlic oil intravenous emulsion.