摘要
目的建立一种新的微乳液相色谱法,同时测定氨酚曲麻片中对乙酰氨基酚、咖啡因、水杨酰胺、盐酸伪麻黄碱、盐酸曲普利啶5种成分的含量。方法通过考察微乳流动相体系中表面活性剂SDS的浓度、油相的种类和浓度、流动相的pH值及β-环糊精的浓度对分离选择性的影响,得到最佳微乳体系的组成,即:质量分数3.0%SDS-质量分数6.0%正丁醇-质量分数0.6%正辛烷-体积分数0.3%三乙胺-10 mmol.L-1β-环糊精-质量分数90%水(磷酸调节pH值至5.0)。色谱条件为Venusil ASB C18柱(4.6 mm×150 mm,5μm),柱温35℃,流速0.7 mL.min-1,分段变波长0~8.0 min 280 nm、8.1~15.0 min 257 nm、15.1 min 233 nm。结果氨酚曲麻片中5种成分在25 min内达到基线分离,5种成分在理论浓度的20%~180%内线性关系良好,相关系数r≥0.999 0,平均回收率98.4%~101.5%。结论微乳液相色谱法比HPLC更经济、简单、快速,可应用于氨酚曲麻片中5种成分的含量分析。
Objective To establish a novel microemulsion system and develop this method for the rapid sim- ultaneous determination of contents of acetaminophen, caffeine, salicylamide, pseudoephedrine hydrochloride and triprolidine hydrochloride in paracetamol triprolidine hydrochloride and pseudoephedrine hydrochloride tablets by microemulsion liquid chromatography (MELC). Methods The effect on the chromatography of va- rious operating parameters was studied, the parameters including the surfactant concentration, the type and concentration of oil phase, the pH of eluent,β-cyclodextrin concentration. MELC was performed on a Venu- sil ASB C18 analytical column( 150 mm ×4. 6 mm,5 μm)at 30 ℃. The optimized MELC system with mi- croemulsion consisted of 3.0% (w) SDS-6. 0% (w) butanol-0. 6% (w) octane-0. 3% (1) triethylamine- 10 mmol.L-1 β-cyclodextdn-90% (w)water, the pH of which was adjusted to 5, 0 with phosphoric acid; The flow rate was set at 0. 7 mL-min- 1 and the samples were measured at multiple wavelengths :0-8.0 min 280 nm,8. 1-15.0 min 257 nm,15, i min 233 nm. Results Rapid separations of five ingredients in paraceta- mol triprolidine hydrochloride and pseudophedrine hydrochloride tablets were achieved in 25 min, The linear- ity established was 20%- 180% of theoretical concentrations of each product in dosage form with r ≥ 0. 999 0 ;The mean recoveries were 98.4% to 101.5%. Conclusions The proposed MELC procedure for the separation of five ingredients in the tablets is less expensive compared with the conventional RP-HPLC meth- od, and it is proved to be a simple and rapid way. The optimized and validated method can be applied to qualitative analysis of five ingredients in the tablets.
出处
《沈阳药科大学学报》
CAS
CSCD
北大核心
2012年第6期456-461,共6页
Journal of Shenyang Pharmaceutical University
基金
国家自然科学基金资助项目(81173525)
关键词
微乳液相色谱
对乙酰氨基酚
咖啡因
水杨酰胺
盐酸伪麻黄碱
盐酸曲普利啶
含量测定
microemulsion liquid chromatography
acetaminophen
caffeine
salicylamide
pseudoephed- rine hydrochloride
tdprolidine hydrochloride
content determination