大蒜油静脉注射乳剂指纹图谱及指标成分含量测定方法研究

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。

Studies on Content Assay and Fingerprints of Intravenous Emulsion Containing Garlic Oil

OBJECTIVE： To establish and a method for determination of allicin and the fingerprints of intravenous emulsion containing garlic oil. METHODS： GC method was applied to determine allicin in preparation and the fingerprints of intravenous emulsion containing garlic oil. The separation was performed on HP-5 （30m×320μm×0.25μm） column with the flow rate of 1.0 mL· min^-1 and inlet temperature of 250 ℃. The column temperature was 60-220℃ and rose by temperature-programmed method with N2 as carrier gas. The temperature of FID detector was 300 ℃ with furan as internal standard. RESULTS： The linear ranges of allicin were 0.05-2.4 mg· min^-1 （r=0.999 8）. The average recovery were 102.5% （RSD=0.41%, n=9）. There were 17 mutual peaks in the fingerprints of intravenous emulsion containing garlic oil. The RSD of intra-day relative retention time and relative peak area were less than 0.05% and 8% respectively. After preparation setting for 48 h at room temperature, the RSD of relative retention time and relative peak areas were less than 0.08% and 15% respectively. The RSD of them in the replicate test were less than 0.04% and 8%, respectively. CONCLUSION： The method is accurate, reliable, simple and available for quality control of intravenous emulsion containing garlic oil