摘要
目的:建立HPLC法对乳酸菌素制剂中L-乳酸和D-乳酸对映体进行拆分,并测定两者在乳酸菌素制剂中的含量与比例,运用L-乳酸和D-乳酸比值对搜集到的样本进行可能的工艺稳定性评价。方法:采用手性柱Chirex 3126(D青霉胺)-Phenomenex(250 mm×4.6 mm,5μm)色谱柱,以2 mmol·L^(-1)硫酸铜溶液-异丙醇(95∶5)为流动相,流速1.0 m L·min^(-1),紫外检测波长254 nm,柱温为30℃。结果:L-乳酸与D-乳酸质量浓度在0.10~1.04 mg·m L^(-1)范围内均呈良好线性(r=0.999 9);平均回收率(n=9)分别为97.5%和98.3%;检测限分别为0.094 4和0.124 6μg·m L^(-1);供试品溶液在48 h内稳定性良好;总体样本L-乳酸和D-乳酸比值在0.93~1.68之间。结论:该方法简单快捷,适合于乳酸菌素制剂中乳酸对映体的含量测定研究,用L-乳酸和D-乳酸比值经统计可以观察样本间离散程度,能反映出各厂间工艺稳定性水平。
Objective: To establish an HPLC method for enantiomer separation of L-lactic acid and D-lactic acid,assay the L-lactic acid and D-lactic acid isomer and their ratios in some lacidophilus preparations and use L-lactic acid and D-lactic acid ratio of the collected samples for possible evaluation of process stability. Methods: The separation was performed on a Chirex 3126( D-penicillamine) chiral column( 250 mm × 4. 6 mm,5 μm) and detected by ultraviolet detector( UV). The detection wavelength was set at 254 nm. The column temperature was set at 30 ℃.The mobile phase consisted of 2 mmol·L-1copper sulfate solution-isopropyl alcohol( 95∶ 5) at a flow rate of 1. 0m L·min-1. Results: The calibration curve of L-lactic acid and D-lactic acid was linear in the range of 0. 10-(-1). 04mg·m L-1( r = 0. 999 9); the average recoveries( n = 9) of the method were 97. 5% and 98. 3%,respectively; the limits of detection were 0. 094 4 μg·m L-1and 0. 124 6 μg·m L-1,respectively; the sample solution was stable within 48 h. The ratio range of L-lactic acid to D-lactic acid in total samples was 0. 93-1. 68. Conclusion: The method is simple,accurate and sensitive,and suitable for the determination of L-lactic acid and D-lactic acid in lacidophilus preparation,and the L-lactic acid and D-lactic acid ratio of the statistical sample can be used to observe the degree of dispersion and reflect process stability level of each pharmaceutical factory.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2015年第12期2126-2130,共5页
Chinese Journal of Pharmaceutical Analysis
基金
2014年国家药品计划抽验(中央补助地方经费项目)品种序号27
关键词
乳酸菌素制剂
手性固定相
乳酸对映异构体
乳酸对映体比值
紫外检测器
L-乳酸
D-乳酸
工艺稳定性评价
lacidophilus preparation
chiral stationary phase
lactic acid enantiomers
ratio of lactic acid enanti-omers
ultraviolet detector(UV)
L-lactic
D-lactic
process stability evaluation