HPLC法测定复方氨酚苯海拉明片中对乙酰氨基酚、咖啡因、盐酸麻黄碱和盐酸苯海拉明的含量

目的建立同一色谱条件测定复方氨酚苯海拉明片中的对乙酰氨基酚、咖啡因、盐酸麻黄碱和盐酸苯海拉明含量的HPLC法。方法采用苯基柱(4.6 mm×250 mm,5μm),流动相为甲醇-pH 3.5的10 mmol.L-1乙酸铵溶液(体积比85∶15),检测波长为225 nm。结果对乙酰氨基酚、咖啡因、盐酸麻黄碱和盐酸苯海拉明的分离度好,对乙酰氨基酚、咖啡因、盐酸麻黄碱和盐酸苯海拉明的回收率分别为100.1%、100.0%、100.2%和100.6%(n=9)。结论本方法操作简单,结果准确,可以有效地控制复方氨酚苯海拉明片的质量。     

复方妥英麻黄茶碱片长期应用致苯妥英中毒出现脑干损害

,维生素B12.1周后患者可独立行走,头晕缓解.     

Simultaneous release of diclofenac sodium and papaverine hydrochloride from tablets and pellets using the flow-through cell apparatus described by dimensionless equations

The release of diclofenac sodium and papaverine hydrochloride from tablets and pellets using the flow-through cell apparatus was studied. The influence of excipients and of a size of the solid dosage forms on the amount of the released substances at the intervals of time using the different rates of flow of the dissolution medium was investigated. Physical parameters corresponding to the dissolution process as the mass transfer coefficient, the thickness of the boundary diffusion layer and the concentration of the saturated solution at this layer were calculated. The results of release were described by dimensionless equations.     

HPLC法测定复方茶碱麻黄碱片中茶碱、咖啡因和可可碱的溶出度

目的:建立高效液相色谱法测定复方茶碱麻黄碱片中可可碱、茶碱和咖啡因的溶出度的方法.方法:采用溶出度测定法(桨法),以水为溶出介质,转速为50 r · min-1,45 min时取样.采用Apollo C18色谱柱(4.6 mm ×250 mm,5 μm),以醋酸盐缓冲液-乙腈(93:7)为流动相,流速0.8 mL · ...     

Assay of ephedrine hydrochloride and theophylline in pharmaceutical formulations by differential-derivative spectroscopy

Rapid and accurate binary mixture resolution of ephedrine hydrochloride and theophylline was performed. Differential-derivative spectrophotometry with a zero-crossing measurement technique was used for the quantitative determination of ephedrine hydrochloride and theophylline in pharmaceuticals. Neither sample pretreatment nor separation were required. Linear calibration graphs of differential first derivative values (at 262.4 and 256.3 nm for theophylline and ephedrine hydrochloride, respectively) versus concentration (in the ranges 6.0-40.0 and 100.0-1000.0 microg ml(-1) for theophylline and ephedrine hydrochloride, respectively) were obtained with negligible intercepts. Vierordt's method was also developed for a comparison method. Commercial tablet and laboratory-prepared mixtures containing both drugs were assayed using the developed methods. Both methods showed good linearity, precision and reproducibility.     

复方妥英麻黄茶碱片致苯妥英中毒4例

4例有哮喘症状的患者,男、女各2例,年龄54～65岁,口服复方妥英麻黄茶碱片4～9片/d,每片含苯妥英钠50mg,每日总剂量为200～450mg,服药时间1～4年。服药期间患者逐渐出现头晕、眼球震颤、步态不稳等症状及小脑性共济失调的体征。检测苯妥英血药浓度34.15～94.12μg/mL,为治疗血药浓度的1.7～4.7倍,诊断为苯妥英钠中毒。停用复方妥英麻黄茶碱片,4～7d后患者中毒症状消失。2例患者复查血药浓度,分别降至1.03、1.14μg/mL。     

HPLC测定止嗽青果片中麻黄碱的含量

目的 采用HPLC测定止嗽青果片的含量.方法色谱柱用C18柱(250 mm× 4.6 mm,5μm),乙腈-0.1%磷酸溶液(5∶95)为流动相,流速1.0 mL· min -,检测波长210 nm.结果盐酸麻黄碱在10.0～50.0 μg·mL-1呈良好的线性关系(r=0.9999),平均回收率为98.8%,RSD=...     

Simultaneous determination of lidocaine hydrochloride, hydrocortisone and nystatin in a pharmaceutical preparation by RP-LC

A liquid chromatographic (LC) method was developed to analyze a formulation (mouthwash) containing lidocaine hydrochloride, hydrocortisone and nystatin. A single LC method with UV detection was developed. A Waters Symmetry C18 HPLC column (150 mm ×  4.6 mm, 5 μm) was used as stationary phase and the assay was performed with gradient elution using mobile phases containing methanol - 0.1 M NaH₂PO₄ with a pH that was previously adjusted to 4.5 with dilute phosphoric acid. The sample pretreatment was performed by treating the formulation with methanol followed by filtration. After method development, the influence of the different chromatographic parameters on the separation, the interference of other active compounds and excipients, linearity, accuracy, repeatability and intermediate precision were investigated. The method was shown to be selective, linear, accurate, precise and repeatable. Finally, the content of the compounds in the formulation was determined.     

Plasma levels of phenobarbital resulting from sustained release tablets containing theophylline,phenobarbital and ephedrine

Plasma levels of phenobarbital were measured in 10 individuals with stable mild to moderate bronchial asthma who were receiving repeated oral doses of a commercial sustained release formulation containing phenobarbital (25 mg), theophylline (180 mg) and ephedrine (48 mg). Following the initial dose, the mean plasma level of phenobarbital was 0.72 μg/ml at 5 h and 0.62 μg/ml at 10 h. After 14 days, during which time the formulation was administered twice daily, the mean phenobarbital plasma level had increased to approximately 4 μg/ml. This value was maintained during 10 h following the last dose.The degree of phenobarbital accumulation in plasma was predictable from previously calculated pharmacokinetic constants, and there was no evidence of autoinduction of phenobarbital metabolism. Phenobarbital is efficiently absorbed from this dosage form and plasma levels of phenobarbital accumulate 3–5 times more than those of theophylline during repeated dosing.     

高效液相色谱法测定麻杏口服液中盐酸麻黄碱及盐酸伪麻黄碱的含量

目的 建立HPLC法测定麻杏口服液中盐酸麻黄碱及盐酸伪麻黄碱的含量。 方法 采用Phenomenex Hydro-RP (250 mm×4.6 mm,4 μm)色谱柱,以乙腈(A)-0.1%磷酸溶液(含0.1%三乙胺)(B)为流动相,梯度洗脱(0~20 min,3%→10% A),流速:1.0 ml/min,检测波长:210 nm,进样量:20 μl。 结果 盐酸麻黄碱在0.99~39.6 μg/ml范围内线性关系良好,r=0.999 9, 平均回收率为101.5%,RSD为1.77%(n=6);盐酸伪麻黄碱在1.09~43.6 μg/ml范围内线性关系良好,r= 0.999 9,平均回收率为100.8%, RSD为 1.96%(n=6)。 结论 本法简便、可靠、准确,可用于该制剂的质量控制。     

HPLC同时测定止嗽定喘丸中的盐酸麻黄碱及盐酸伪麻黄碱

目的 建立止嗽定喘丸中盐酸麻黄碱与盐酸伪麻黄碱的含量测定方法.方法 采用固相萃取技术处理样品,HPLC测定,色谱柱为Shim - pack VP - ODS C18(150mm×4.6mm,5μm),流动相为乙腈-0.1％磷酸溶液(5∶95),检测波长210 nm,流速1 mL· rain-l.结果 4.41～147.0 μg·mL-1盐酸麻黄碱、2.33 ～116.6 μg·mL-1盐酸伪麻黄碱与峰面积的线性关系良好(r=0.9999),回收率分别为100.02％、97.73％(n=9).结论　所用方法准确可靠、重复性好,可作为止嗽定喘丸的质量控制.     

Determination of theophylline and ephedrine HCL in tablets by ratio-spectra derivative spectrophotometry and LC

Two methods are described for the determination of theophylline (THP) and ephedrine hydrochloride (EPH) in combined pharmaceutical tablet forms. The first method depends on the use of the first derivative of the ratio-spectra obtained by dividing the absorption spectrum of binary mixtures by a standard spectrum of one of the compounds. The first derivative amplitudes at 231.8 and 250.3 nm were selected for the assay of THP and EPH, respectively. Calibration graphs were established for 20-180 microg ml(-1) for THP and 10-50 microg ml(-1) for EPH. The second method is based on high-performance liquid chromatography on a reversed-phase column using a mobile phase of methanol-water (40+60,v/v) (pH 3) with detection at 217 nm. Linearity was obtained in the concentration range of 5-150 microg ml(-1) for THP and 15-75 microg ml(-1) for EPH. The detection limits for THP and EPH were 0.73 and 0.92 microg ml(-1) by ratio-spectra derivative spectrophotometry and 0.59 and 0.86 microg ml(-1) by HPLC, respectively. The proposed methods were successfully applied to the determination of these drugs in laboratory-prepared mixtures and in tablets. The relative standard deviations were found to be less than 1.5%, indicating reasonable repeatibility of both methods.     

高效液相色谱法同时测定三拗片中盐酸麻黄碱和苦杏仁苷的含量

目的建立高效液相色谱同时测定三拗片中盐酸麻黄碱和苦杏仁苷含量的方法。方法采用Hypersil BDSC18柱(250 mm×4.6 mm,5μm),流动相为甲醇-0.3%磷酸溶液(20∶80),检测波长为217 nm,流速为1.0 mL.min-1,柱温为30℃,外标法计算含量。结果盐酸麻黄碱在0.019 9~0.398μg与峰面积有良好的线性关系,r=0.999 8,平均回收率为97.6%,RSD为1.2%(n=9);苦杏仁苷在0.104 2~2.084μg与峰面积有良好线性关系,r=0.999 9,平均回收率为98.2%,RSD为1.0%(n=9)。结论该方法简便、准确、重复性好,可同时测定三拗片中盐酸麻黄碱和苦杏仁苷的含量。     

0.5%盐酸麻黄碱滴鼻液含量测定方法研究

目的　建立 0 .5 %盐酸麻黄碱滴鼻液的含量测定方法。方法　比较旋光度法 ,酸碱滴定法 ,两种测定 0 .5 %盐酸麻黄碱滴鼻液的方法 ,挑选一种最佳的含量测定方法。结果　旋光度法在 2 .5～ 2 0mg/mL之间线性关系良好 (r=0 .99998) ,平均回收率为 10 0 .8% ,RSD =0 .0 5 4 %。结论　旋光度法简便快速 ,结果可靠可用于测定 0 .5 %盐酸麻黄碱滴鼻液。     

Microbiological assay for terbinafine hydrochloride in tablets and creams

The optimization of a microbiological assay, applying the cylinder-plate method, for the determination of the antifungal terbinafine hydrochloride is described. Using a strain of Aspergillus flavus ATCC 15546 as the test organism, terbinafine hydrochloride at concentrations ranging from 0.125 to 0.5 microg ml(-1) could be measured in tablets and creams. A prospective validation of the method showed that the method was linear (r=0. 9999), precise (intra-day: CV=0.48%-tablets and 0.43%-creams; inter-day: CV=0.98%-tablets and 0.64%-creams) and accurate (it measured the added quantities). The method shows results that confirm its precision, not differing significantly the others methods described in the literature. We conclude that the microbiological assay is satisfactory for quantitation of in vitro antifungal activity of terbinafine.