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目的:利用气相色谱法建立一种测定双氯芬酸钠原料中甲苯残留量的检测方法。方法:采用HP-5(0.53 mm×30 m,2.65μm)毛细管柱,载气为N2,FID检测器。采用等温法,柱温50℃,进样口温度200℃,检测器温度250℃,分流直接进样,二甲亚砜(DMSO)为溶剂,异辛烷为内标物,内标法计算甲苯残留溶剂的含量。结果:甲苯在9.27~111.19μg·ml-1的范围内线性关系良好(r=0.999 4),平均回收率为97.27%(RSD=2.80%,n=9),检测限(LOD)和定量限(LOQ)分别为0.59μg·ml-1和1.46μg·ml-1。3批样品检测甲苯残留均未超标。结论:该方法结果准确可靠,可用于双氯芬酸钠原料的质量控制。
Objective: To establish a method for the determination of toluene residues in diclofenac sodium by gas chromatography. Methods: HP-5 (0.53 mm × 30 m, 2.65 μm) capillary column was used. The carrier gas was N2 and FID detector. The isothermal method was used, the column temperature was 50 ℃, the inlet temperature was 200 ℃, the detector temperature was 250 ℃. The direct injection of split stream, dimethyl sulfoxide (DMSO) as solvent and isooctane as internal standard, Residual solvent content. Results: The linear range was 9.27 ~ 111.19μg · ml-1 (r = 0.999 4) and the average recovery was 97.27% (RSD = 2.80%, n = 9). The limit of detection (LOD) and limit of quantification (LOQ) were 0.59μg · ml-1 and 1.46μg · ml-1.3 batch of toluene residues were not exceeded. Conclusion: The method is accurate and reliable and can be used for the quality control of diclofenac sodium.