摘要
以在线扫集-胶束毛细管电动色谱法(Sweeping-MEKC)测定了复方氨酚烷胺胶囊中的马来酸氯苯那敏、咖啡因和对乙酰氨基酚3种有效成分。考察了缓冲溶液pH值、SDS浓度、分离电压及进样时间等对分离效果的影响。优化条件:以未涂层熔融石英毛细管(55 cm×50μm,有效柱长35 cm)为分离柱;环境温度25℃;80 mmol/L十二烷基磺酸钠+20 mmol/L NaH2PO4(pH 2.2)+15%乙腈为缓冲体系,分离电压-20kV,进样时间60 s(H=20.0 cm),测量波长210 nm。在该条件下氯苯那敏、咖啡因和对乙酰氨基酚在25min内出峰,峰面积RSD均小于4%;线性范围分别为2.45~39.17、1.61~25.76、1.58~25.28 mg/L;检出限(S/N=3)分别达139、34、24μg/L,回收率分别为96%~101%、98%~102%、96%~102%。
A sweeping -micellar electrokinetic chromatographic (sweeping- MEKC ) method was used for the simultaneous separation and determination of ehlorphenamine maleate, caffeine and aeet- aminophen in compound paracetamol and amantadine hydrochloride capsules. Effects of sodium dode- cyl sulfate(SDS) concentration, separation voltage, injection time of sample, composition and con- centration of background buffer on separation efficiency were optimized. An optimal separation of three compounds was obtained on an uncoated fused silica capillary column( 50 em x 50 μm, effec- tive length 35 cm) by using background buffer containing 80 mmol/L SDS, 20 mmoL/L NaH2PO4 and 15% acetonitrile at pH 2.2 with a constant temperature of 25 ℃. The detection wavelength was set at 210 nm, the separation voltage at -20 kV and the sample injection time for 60 s. The result indica- ted that the separation of three compounds was performed within 25 min with relative standard devia- tion(RSDs) of their peak areas less than 4% . The calibration curves showed good linearities in the ranges of 2.45 -39. 17 mg/L for chlorphenamine, 1.61 -25.76 mg/L for caffeine and 1.58 -25.28 mg/L for aeetaminophen, with detection limits(S/N = 3) of 139, 34, 24 μg/L, respectively. The spiked recoveries for acetaminophen, caffeine and ehlorphenamine maleate were 96% -101%, 98% - 102% and 96% - 102% , respectively.
出处
《分析测试学报》
CAS
CSCD
北大核心
2012年第3期284-289,共6页
Journal of Instrumental Analysis
基金
桂科自资助项目(0832062)