香茅醇亚微乳的处方工艺优化研究

目的:优化香茅醇亚微乳的制备工艺。方法:采用高效液相色谱法测定香茅醇亚微乳中的香茅醇含量;采用高速剪切分散-高压均质法制备香茅醇亚微乳,以离心稳定常数(ke)、粒径为指标,对其处方及工艺进行优化并进行验证;测定所得制剂的载药量的包封率。结果:香茅醇检测质量浓度的线性范围为4～64μg/mL(R²=0.999 9);精密度、稳定性(24 h)、重复性试验的RSD均小于3%;加样回收率为97.64%～101.97%(RSD=2.28%,n=3)、97.71%～99.50%(RSD=1.29%,n=3)、96.87%～101.48%(RSD=2.86%,n=3)。最优处方为大豆油+中链甘油三酯(1∶1,g/g)总质量3.75 g,1.2%大豆磷脂0.6 g,胆固醇0.06 g,香茅醇1.25 g,0.6%油酸钠0.3 g,15-羟基硬脂酸聚乙二醇酯0.75 g,泊洛沙姆188 0.75 g,加水至50 mL。最优工艺为于4℃下以13 000 r/min高速剪切5 min制得初乳后,经稀盐酸调p H至7,再以600 Bar高压均质5 min。按最优处方及工艺制备的3批香茅...

Study on Optimization of Formulation and Technology of Citronellol Submicroemulsion

OBJECTIVE:To optimize the preparation technology of citronellol submicroemulsion.METHODS:The content of citronellol in Citronellol submicroemulsion was determined by HPLC.Citronellol submicroemulsion by high-speed shearing dispersion-high pressure homogenization method,with centrifugation stability constant(ke)and particle size were used as evaluation indexes.Its formulation and preparation technology were optimized and validated.Drug-loading amount and encapsulation rate of the preparation were detected.RESULTS:The linear range of citronellol were 4-64μg/mL(R 2=0.9999).RSDs of precision,stability(24 h)and reproducibility tests were all lower than 3%.The recoveries were 97.64%-101.97%(RSD=2.28%,n=3),97.71%-99.50%(RSD=1.29%,n=3),96.87%-101.48%(RSD=2.86%,n=3).The optimal formulation included that total weight of soybean oil and medium chain triglycerides(1∶1,g/g)was 3.75 g,1.2%soybean phospholipid was 0.6 g,cholesterol was 0.06 g,citronellol was 1.25 g,0.6%sodium oleate was 0.3 g,15-hydroxystearic acid polyethylene glycol ester was 0.75 g,poloxamer 188 was 0.75 g,water added to 50 mL.After prepared by optimal technology at 4℃which contained shearing speed of 13000 r/min,lasting for 5 min,primary emulsion was adjusted to pH 7 with dilute hydrochloric acid,and homogenized with 600 Bar high pressure for 5 min.The parameters of Citronellol submicroemulsion according to optimal formulation and technology contained mean particle size of(91.05±0.26)nm,PDI of(0.20±0.01),Zeta-potential of(-30.86±0.39)mV,average content of citronellol(100.21±0.01)%,the drug-loading amount was(2.4817±0.0007)mg/mL,the encapsulation rate was(99.27±0.03)%.CONCLUSIONS:The optimal formulation and technology is stable and feasible.