摘要
目的建立左乙拉西坦原料药中痕量相转移催化剂测定的离子色谱方法。方法四丁基溴化铵为离子化合物而左乙拉西坦水溶性较好,故选离择子色谱法测定。本方法以Dionex IonPac SCS1阳离子交换色谱柱为分析柱,5 mmol/L甲烷磺酸溶液(含乙腈35%)为淋洗液,直接进样法测定。通过条件的优化,本方法以抑制电导检测降低背景噪音,同时增大供试液浓度(50 mg/ml)及进样体积(200μl)提高方法检测灵敏度,使得方法满足了痕量测定的要求。结果样品基质及常见阳离子对测定无干扰,四丁基溴化铵在0.1μg/ml^5.0μg/ml范围内线性关系良好(r=0.9999),最低检出限为0.05μg/ml,平均回收率为99.2%(n=9,RSD=3.6%)。方法进样重现性良好,其中保留时间RSD为0.07%(n=5),峰面积RSD为0.72%(n=5)。结论方法操作简单,灵敏度高,重复性好,可用于水溶性药品中痕量阳离子的检测。
Objective To establish a ion chromatographic method for determination of residual phase transfer catalyst in phar- maceutical ingredient. Methods Considering tetrabutyl ammonium bromide was ionic compound and levetiracetam was water - soluble, so ion chromatography determination was the first choice. The Dionex IonPac SCS1 was used as analytical column with 5 mmol/L methanesulfonic acid （including 35% acetonitrile） as the mobile phase. Besides, Dionex ASRS4mm as suppressor conductivity detector was used to reduce background noise, the concentration of test solution（50 mg/ml） and the direct injection volume （200 pL1） were augmented to improve sensitivity. Results The sample matrix and common cation showed no interference in determination of pharmaceutical ingredient. Tetrabutyl ammonium bromide was linear in the range of 0.1 μg,/ml N 5.0 μg/ml （ r = 0. 9999）. The average recovery of tetrabutyl ammonium bromide was 99.2% （ n = 9, RSD = 3.6% ）. The detection limit of this method can reach 0.05 μg/ml. Reproducibility of this method was good, the RSD of retention time was 0.07% （n = 5）, and that of peak area was 0.72% （ n = 5）. Conclusion The developed method is simple, sensitive and repeatable, it can be applied to detect the trace cation in water- soluble pharmaceutical ingredient.
出处
《中国卫生检验杂志》
北大核心
2014年第4期505-507,共3页
Chinese Journal of Health Laboratory Technology
关键词
左乙拉西坦
四丁基溴化铵
离子色谱
痕量分析
Levetiracetam
Tetrabutyl ammonium bromide
Ion chromatography
Trace analysis
