摘要
目的:建立采用邻苯二甲醛(O-phthaldialdehyde,OPA)作为柱后衍生试剂的HPLC法测定门冬氨酸鸟氨酸颗粒的有关物质与含量。方法:采用色谱柱Synergi Hydro RP,C18(150 mm×3 mm,4μm),流动相A为0.005 mol/L辛烷磺酸钠溶液-高氯酸(100∶0.16),流动相B为0.01 mol/L辛烷磺酸钠溶液-乙腈-高氯酸(50∶50∶0.16),进行梯度洗脱;检测波长为336 nm。结果:门冬氨酸和鸟氨酸在37.5~112.5μg/ml范围内,浓度与峰面积呈良好的线性关系(门冬氨酸r=0.999 8,鸟氨酸r=0.999 9);门冬氨酸回收率为101.2%,RSD为0.92%(n=9),鸟氨酸回收率为101.0%,RSD为0.97%(n=9);门冬氨酸鸟氨酸主成分峰与3种杂质峰分离度均符合要求,门冬氨酸和鸟氨酸最低检出限均为5ng。结论:该方法方便、快速、灵敏度高、重现性好,适用于测定门冬氨酸鸟氨酸颗粒剂中的有关物质及含量。
Objective: A HPLC with 0 -phthaldialdehyde (OPA) postcolumn derivatization was developed to determine thecontent of ornithine aspartate granules and its related substances. Methods: The HPLC method was applied with a Synergi Hydro RP C18 column( 3 mm ×150 mm, 4 μm) by a gradient elution. The mobile phase A was consisted of 0.005 mol/L 1 - Octanesulfonic acid sodium salt- perchloric acid (100: 0.16), the mobile phase B was consisted of 0.01 mol/L 1 -Octanesulfonic acid sodium salt- acetonitrile - perchloric acid C 50: 50: 0.16). The detection wavelength was set at 336 nm. Results: The linear range of ornithine and aspartate was 37.5 - 112.5 μg/ml ( r = 0. 999 8 and 0. 999 9 for aspartate and omithine, respectively ). The recovery rate of aspartate was 101.2%, RSD was 0.92% ( n = 9 ) , and the recovery rate of ornithine was 101.0% , RSD was 0.97% ( n = 9 ). The detection limit for ornithine and aspartate were both 5 ng. Conclusion: This method is simple, rapid, sensitive, reproducible, accurate and reliable, and it is suitable for the detection of the content and related substances of ornithine aspartate granules.
出处
《天津药学》
2011年第5期4-7,共4页
Tianjin Pharmacy