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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 the separation of L-lactic acid and D-lactic acid enantiomers from lactic acid bacteriocin preparations and to determine their content and proportion in lactobacillus preparations. Using L-lactic acid and D-lactic acid ratio, Of the samples for potential process stability evaluation. Methods: The chiral column Chirex 3126 (D penicillamine) -Phenomenex (250 mm × 4.6 mm, 5 μm) was used in this study. The extraction was performed with 2 mmol·L -1 CuSO 4 -isopropanol (95: 5) As the mobile phase at a flow rate of 1.0 m L · min -1. The UV detection wavelength was 254 nm and the column temperature was 30 ℃. RESULTS: The linear range of L-lactic acid and D-lactic acid was 0.10-1.04 mg · mL -1 (r = 0.999 9), and the average recoveries (n = 9) were 97.5% and The detection limits were 0.094 4 and 0.124 6 μg · m L -1, respectively. The stability of the test solution was good within 48 h. The ratio of L-lactic acid to D-lactic acid in the whole sample ranged from 0.93 to 1.68. Conclusion: The method is simple and rapid, suitable for the determination of lactic acid enantiomer in lactic acid bacteriocin preparations, L-lactic acid and D-lactic acid ratio statistics can observe the degree of dispersion between samples can reflect the process of plant stability level .