论文部分内容阅读
目的:建立了HPLC法测定六甲蜜胺有关物质及胶囊剂的含量。方法:采用Agilent 1100型高效液相色谱仪,色谱柱为Kromasil C_(18)(4.6 mm×250 mm,5μm)柱,流动相为甲醇-碳酸铵溶液[取碳酸铵0.79 g,加水1000 mL使溶解,用甲酸溶液(1→10)或氨水溶液(1→10)调节pH至8.0±0.05](75:25),流速1.0 mL·min~(-1),检测波长227 nm,柱温:40℃。结果:六甲蜜胺有关物质线性范围为0.0253～1.517μg·mL~(-1)(r=0.9999),杂质限度范围为0.05%～3.0%,最低检测限为0.125 ng(0.025%);六甲蜜胺胶囊含量测定线性范围为12.56～75.35μg·mL~(-1)(r=0.9998),平均回收率为99.8%,RSD=0.7%(n=9)。结论:该方法准确、灵敏、重现性好,专属性强,可用于六甲蜜胺及其胶囊的质量控制。
Objective: To establish a HPLC method for the determination of altretamine related substances and capsules. Methods: Agilent 1100 HPLC was used. The column was Kromasil C18 (4.6 mm × 250 mm, 5 μm). The mobile phase consisted of methanol-ammonium carbonate solution [0.79 g of ammonium carbonate and 1000 mL of water The solution was adjusted to pH 8.0 ± 0.05 with formic acid solution (1 → 10) or ammonia solution (1 → 10) at a flow rate of 1.0 mL · min -1. The detection wavelength was set at 227 nm. Column temperature: 40 ° C. Results: The linear range of altretamine was 0.0253-1.517μg · mL -1 (r = 0.9999), the limit of impurity was 0.05% -3.0%, the lowest limit of detection was 0.125 ng (0.025%), The linear range was 12.56 ~ 75.35μg · mL -1 (r = 0.9998). The average recovery was 99.8%. The RSD was 0.7% (n = 9). Conclusion: The method is accurate, sensitive, reproducible and specific. It can be used for quality control of melatonin and its capsules.