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目的:建立磷酸泰乐菌素脂质体中药物含量及包封率测定的RP-HPLC法。方法:采用Kromasil C18柱(4.6mm×150mm,5μm),流动相:0.05mol.L-1高氯酸钠溶液(用1mol.L-1盐酸调节pH至3.0±0.1)-乙腈(65∶35),流速:1.0mL.min-1,紫外检测波长:290nm,柱温:30℃,进样量:20μL。采用低温高速离心法(4℃,12000r.min-1,45min)分离磷酸泰乐菌素脂质体与游离药物,测定包封率。结果:在所选定的色谱条件下,磷酸泰乐菌素各组分峰与辅料及溶剂峰分离良好,磷酸泰乐菌素在5.0~320.0μg.mL-1浓度范围内与峰面积呈良好线性关系(r=0.9999,n=7),回收率在99.9%~100.1%之间(n=5),日内RSD及日间RSD均小于2%(n=5)。低温高速离心法对游离药物的回收率为99.4%~101.4%,RSD均小于2%(n=3)。结论:该方法准确可靠、方便快捷,可用于磷酸泰乐菌素脂质体中药物含量及包封率的测定。
Objective: To establish a RP-HPLC method for the determination of drug content and entrapment efficiency of tylosin phosphate liposomes. METHODS: Kromasil C18 column (4.6 mm × 150 mm, 5 μm) was used. The mobile phase consisted of 0.05 mol·L-1 sodium perchlorate solution (pH adjusted to 3.0 ± 0.1 with 1 mol·L- ), Flow rate: 1.0mL.min-1, UV detection wavelength: 290nm, column temperature: 30 ℃, injection volume: 20μL. Low temperature and high speed centrifugation (4 ℃, 12000r.min-1, 45min) separation of tylosin phosphate liposomes and free drugs, determination of entrapment efficiency. Results: Under the selected chromatographic conditions, the components of tylosin phosphate were separated well from the excipients and solvent peaks. The content of tylosin phosphate was good with the peak area in the range of 5.0-320.0 μg.mL-1 The linear relationship was obtained (r = 0.9999, n = 7). The recoveries ranged from 99.9% to 100.1% (n = 5). The intraday RSD and daytime RSD were less than 2% (n = 5). The recovery rate of free drug by low temperature and high speed centrifugation was 99.4% ~ 101.4% with RSD less than 2% (n = 3). Conclusion: The method is accurate, reliable and convenient. It can be used for the determination of drug content and entrapment efficiency of tylosin phosphate liposomes.