固相萃取-高效液相色谱法测定复方甲硝唑阴道栓中甲硝唑和盐酸四环素的含量

SPE-HPLC determination of metronidazole and tetracycline hydrochloride in compound metronidazole vaginal suppositories

目的:采用固相萃取-高效液相色谱法分析复方甲硝唑阴道栓中甲硝唑和盐酸四环素的含量。方法:采用C18固相萃取小柱分离除去复方甲硝唑阴道栓中的基质,高效液相色谱法测定甲硝唑和盐酸四环素的含量。色谱柱为Luna C8(5μm,4.6mm×250mm);流动相为0.1mol.L-1草酸铵溶液-二甲基甲酰胺-0.2mol.L-1磷酸氢二铵溶液(65:30:5),检测波长为270nm,流速为1.0mL.min-1。结果:甲硝唑进样量在0.228～2.28μg,盐酸四环素进样量在0.0121～0.121μg范围内,线性关系良好;平均回收率(n=9)甲硝唑为98.8%,盐酸四环素为98.3%。结论:本方法灵敏快速,结果准确,重现性好,可用于该制剂的质量控制。

Objective：To establish SPE - HPLC for determination of metronidazole and tetracycline hydrochloride in compound metronidazole vaginal suppositories. Methods： The sample was purified with C18 solid phase column and its content was determined with HPLC method. The Luna C8 column （5 μm,4. 6 mm × 250 mm）was used and mobile phase was composed of 0. 1 mol · L^-1 ammonium oxalate -N, N- dimethylformamide -0. 2 mol · L^-1 ammonium phosphate dibasic diammonium hydrogen phosphate at a flow rate of 1.0 mL · min^-1. The UV detector wavelength was 270 nm. Results：The linear ranges were 0. 228 -2.28 μg for metronidazole and 0. 0121 -0. 121 μg for tetracycline hydrochloride ;The average recoveries（ n = 9 ）were 98.8% for metronidazole and 98.3% for tetracycline hydrochloride. Conclusion： The method is simple, quick, sensitive, accurate, repeatable and be used to control the quality of compound metronidazole vaginal suppositories.