GC测定白芍总苷原料药中有机溶剂残留

Determination of Residual Solvents in Total Glucosides of Paeony Raw Material Drug by GC

关键词:  白芍总苷  气相色谱法  残留溶剂

Key words:  total glucosides of Paeony  gas chromatography (GC)  residual solvent

摘要:

目的 采用GC同时测定白芍总苷原料药中乙醇、乙酸乙酯和正丁醇3种残留溶剂。方法 检测器为氢火焰离子化检测器（FID），色谱柱为Agilent DB-624石英毛细管柱（30 m×0.53 mm，3.0 μm），溶剂为N，N-二甲基甲酰胺（DMF），程序升温。结果 3种残留溶剂均能完全分离，乙醇、乙酸乙酯和正丁醇分别在24.60~491.98 μg·mL^-1（r=0.999 8），21.01~420.25 μg·mL^-1（r=1.000 0），23.37~467.48 μg·mL^-1（r=0.999 8）内与峰面积呈良好的线性关系，检测限分别为0.002 37%，0.000 08%和0.000 63%。结论 该方法简单可靠，灵敏度高，可用于白芍总苷原料中的残留溶剂控制。

Abstract:

OBJECTIVE To establish a GC method for the content determination of three residual solvents (ethanol, ethyl acetate and N-butanol) in total glucosides of Paeony raw material. METHODS The experiment was carried out by GC with a detector for the hydrogen flame ionization detector (FID) and the column for the Agilent DB-624 capillary column (30 m×0.53 mm, 3.0 μm). The sample was dissolved in DMF solvent. Program temperature was used in the whole process. RESULTS Three residual solvents were separated completely, the linear ranges of ethanol, ethyl acetate and N-butanol were 24.60-491.98 μg·mL^-1 (r=0.999 8), 21.01-420.25 μg·mL^-1 (r=1.000 0) and 23.37-467.48 μg·mL^-1 (r=0.999 8), respectively. The limit of detection was 0.002 37%, 0.000 08% and 0.000 63%. CONCLUSION The method is simple, sensitive and accurate for the quality control of residual solvents in total glucosides of Paeony raw material.