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目的建立顶空毛细管气相色谱法测定非诺贝酸中8种残留溶剂含量的方法。方法色谱柱为Agilent DB-624毛细管柱,采用程序升温,检测器为氢火焰离子化检测器,检测器温度为260℃,以二甲基亚砜为溶剂,外标法计算残留溶剂的含量。结果乙醇、丙酮、异丙醇、二氯甲烷、乙酸乙酯、三氯甲烷、N,N-二甲基甲酰胺和氯苯色谱峰均能得到有效分离,分析时间为13 min;所测残留溶剂在各自的质量浓度范围内呈良好的线性关系(r=0.999 3~0.999 9,n=5);平均回收率在99.3%~101.6%内(RSD=1.4%~2.7%);定量限分别为0.65、0.12、0.50、0.47、0.12、1.20、0.18和0.09 mg·L-1;6批样品中有机溶剂残留量均符合《药品注册的国际技术要求》。结论本方法可用于非诺贝酸中有机溶剂残留量的检测。
Objective To establish a method for the determination of 8 residual solvents in fenofibrate by headspace capillary gas chromatography. Methods The column was an Agilent DB-624 capillary column. The temperature was programmed and the detector was hydrogen flame ionization detector. The temperature of the detector was 260 ℃. The content of residual solvent was calculated by external standard method using dimethyl sulfoxide as solvent. Results The chromatographic peaks of ethanol, acetone, isopropanol, methylene chloride, ethyl acetate, chloroform, N, N-dimethylformamide and chlorobenzene could all be separated effectively with the analysis time of 13 min. The average recoveries were within 99.3% ~ 101.6% (RSD = 1.4% -2.7%). The limits of quantification 0.65, 0.12, 0.50, 0.47, 0.12, 1.20, 0.18 and 0.09 mg · L -1, respectively. The residues of organic solvents in 6 batches of samples all met the international technical requirements of drug registration. Conclusion This method can be used for the determination of residual organic solvents in fenofibrate.