目的:对气相色谱法测定棕榈酸与硬脂酸进行改进,建立无衍生化气相色谱法测定药用胶塞中棕榈酸与硬脂酸的可提取量和迁移量的分析方法。方法:采用DB-FFAP 毛细管色谱柱(30 m× 0.25 mm×0.25 μm);程序升温: 初始温度为100 ℃,保持 1 min,以60 ℃·min-1的速率升至230 ℃,保持20 min;进样口温度250 ℃;氢火焰离子化检测器,检测器温度250 ℃;分流比10∶1;载气流速为1.0 mL·min-1。结果:棕榈酸和硬脂酸线性范围分别为0.884 4～88.44 μg·mL-1(r2=0.999 9) 和1.234～123.4 μg·mL-1(r2=0.999 8),检测下限分别为0.442和0.617 μg·mL-1,回收率分别为96.5%和91.3%。胶塞中棕榈酸和硬脂酸含量分别为0.019%和0.020%,药品中棕榈酸和硬脂酸迁移量均小于安全阈值。结论:该方法样品前处理操作简单,效率高耗时短,无需使用大量危险和有毒试剂,灵敏度高,重复性好,可用于胶塞中棕榈酸与硬脂酸向注射用头孢唑肟钠中可提取量和迁移量的测定。
Objective: To improve gas chromatographic (GC) method for the determination of palmitic acid and stearic acid, and to establish a non-derivative GC method for determining the extracted amount and migration amount of palmitic acid and stearic acid in medicinal rubber stopper. Methods: A DB-FFAP capillary column (30 m×0.25 mm, 0.25 μm) was used and column temperature was programmed heating up. The initial temperature was kept at 100 ℃ for 1min, then the temperature was raised to 230 ℃ at the rate of 60 ℃·min-1 and kept for 20 min. The inlet temperature was 250 ℃, FID detector temperature was 250 ℃, the split ratio was 10∶1 and the carrier gas flow rate was 1.0 mL·min-1. Results: The linear ranges of palmitic acid stearic acid were 0.884 4-88.44 μg·mL-1 (r2=0.999 9) and 1.234-123.4 μg·mL-1(r2=0.999 8), respectively, and the lower limit of detection were 0.442 and 0.617 μg·mL-1, respectively, with the recoveries of 96.5% and 91.3%, respectively. The content of palmitic acid and stearic acid in rubber plug was 0.019% and 0.020%, respectively, and the migration of palmitic acid and stearic acid in medicine was lower than the safety threshold. Conclusion: The sample pretreatment is simple, efficient, rapid and dispense with lots of dangerous and toxic reagents. The method is sensitive and accurate with good repeatability. The validation results show that the method can be used to determine the migration of palmitic acid and stearic acid from rubber stopper to ceftizoxime sodium for injection.
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