注射用水飞蓟宾脂质纳米乳中水飞蓟宾含量测定

Determination of silybin content in silybin lipid nanoemulsion

目的 建立直接紫外分光光度法 ,测定最新研制的注射用水飞蓟宾脂质纳米乳中水飞蓟宾含量的方法。方法 选用 1mol·L-1的NaOH碱溶液破乳 ,弃去以氯仿为萃取剂提取的纳米乳油相 ,水相层由纳米乳中释放出的水飞蓟宾以无水乙醇溶解 ,HCl中和 ,于 2 88nm处直接测定吸光度 ,计算水飞蓟宾的含量。结果 水飞蓟宾在 0 .2 970～ 1.784mg·mL-1浓度范围内呈线性 ,r =0 .9999;高、中、低 3种浓度的萃取回收率和方法回收率分别为 96 .0 8%～ 98.95 %和 99.72 %～ 10 0 .5 % ,n =3;日内和日间RSD分别为 0 .37%和 3.6 % ,n =5。结论 建立的方法准确度高 ,重现性好 。

OBJECTIVE: To develop an ultraviolet spectrophotometry method for the assay of silybin in silybin lipid nanoemulsion. METHODS: Oil phase and other excipients in lipid nanoemulsion were treated with 1 mol&middotL-1 NaOH, followed by extraction with chloroform. Dehydrated alcohol and 1 mol&middotL-1 HCl were added to the aqueous phase containing silybin. The concentration of silybin in lipid nanoemulsion was determined by spectrophotometry at 288 nm. RESULTS: It showed a linear correlation (r = 0.999 9) over the concentration range of 0.297 0∼1.784 mg&middotmL-1. The extraction recoveries and method recoveries of silybin were 96.08% ∼ 98.95% and 99.72%∼100.5% (n = 3), respectively. The RSD of intra- and inter-day were 0.37% and 3.6% (n = 5), respectively. CONCLUSION: The method is accurate and reproducible. It can be used for the quality control of silybin lipid nanoemulsion.