磷酸可待因在Nafion修饰玻碳电极上的伏安行为研究及测定

用循环伏安法和微分脉冲吸附伏安法对磷酸可待因在Nafion修饰玻碳电极上的伏安行为进行了研究。结果表明在 0 .1mol/LHCl底液中 ,磷酸可待因在 + 1 .0 6V处 (vs.SCE)产生一良好的氧化峰 ,磷酸可待因浓度在 5 .0× 1 0 - 7～2 .5× 1 0 - 5mol/L范围内与峰电流呈线性关系 ,检出限为 1 .3× 1 0 - 7mol/L。并分别对其单方药和复方药制剂进行了测定     

磷酸可待因在安伯来特IRP-69上的离子交换平衡特性研究

采用批式离子交换法研究了磷酸可待因在安伯来特IRP-69上的离子交换平衡特性、动力学及热力学特征.结果表明,在3个温度(298K、308K和318K)及研究的浓度范围内,离子交换吸附等温方程和Freundlich方程都能够对磷酸可待因在安伯来特IRP-69上的离子交换平衡等温线进行很好的拟合,其离子交换动力学特征基本符合二级动力学方程.磷酸可待因在安伯来特IRP-69上的离子交换行为的热力学参数(ΔH、ΔG、ΔS)都小于0.在3个温度(298K、308K和318K)下,同一初始浓度(350mmol/L)的磷酸可待因在安伯来特IRP-69上的平衡交换吸附量分别为1.1295mmol/g、1.1203 mmol/g和1.1129 mmol/g.     

CPA矩阵法和多波长线性回归法测定舒尔芬中双氯芬酸钠和磷酸可待因

舒尔芬为双氯芬酸钠和磷酸可待因的复方片剂 ,具有镇痛、抗炎、解热作用 ,适用于各种手术后疼痛。舒尔芬片剂中双氯芬酸钠和磷酸可待因不经分离同时测定的方法未见报道。本文报道用多波长线性回归法 ( MWL)和 CPA矩阵法 ( CPA) ,不经分离同时测定舒尔芬片剂中双氯芬酸钠和磷酸可待因的含量 ,用 BASIC语言编制计算程序 ,方法简便、快速。     

磷酸可待因的振动光谱研究

运用密度泛函理论(DFT)计算了磷酸可待因的拉曼和红外光谱.采用B3LYP混合泛函和6-31G基函数组,同时在实验上测量了磷酸可待因的常规拉曼光谱(NRS)和红外吸收光谱(IRS),结果表明:在振动频率上理论结果与实验结果相当一致,根据理论计算的结果对磷酸可待因的振动光谱进行分析,通过理论与实验数据的比较,对磷酸可待因的所有振动谱带进行了全面地归属.     

胶束扫集毛细管电泳快速测定止咳露中的麻黄碱和可待因

采用胶束扫集毛细管电泳, 建立了快速测定止咳露中麻黄碱和可待因含量的方法, 并通过日间实验、柱间实验等对方法的稳定性进行了考察研究.胶束扫集电动色谱缓冲体系含60 mmol/L 十二烷基磺酸钠, 10 mmol/L NaH2PO4 (pH 2.20), 18%乙腈(V/V), 分离电压-14 kV, 测量波长200 nm. 讨论了pH、 SDS浓度、样品溶剂等对分离效果的影响. 在优化条件下, 麻黄碱和可待因均在5 min内出峰, 方法检出限(μg/mL)、线性范围(μg/mL)、相关系数分别为: 麻黄碱 0.433、 1.73～27.7、 0.9997, 可待因0.833、 3.33～50.3、 0.9996, 回收率在96.7%～103.5%之间. 峰面积日内RSD≤4.2% (n=5), 日间RSD≤8.0% (n=5), 柱间实验RSD≤2.3% (n=3).     

胶束电动毛细管色谱法测定穿心莲中穿心莲内酯和脱水穿心莲内酯

采用胶束电动毛细管色谱法分离测定了中药穿心莲中穿心莲内酯和脱水穿心莲内酯。电泳条件 :以2 0mmol L磷酸缓冲溶液 1 0mmol LSDS(含 5 %甲醇 ,V/V ,pH 6.8)为电泳介质 ,未涂层石英毛细管 (75 μmi.d.× 5 0cm ,有效分离长度 4 2 .2cm)为分离通道 ,压力进样 (2 5 0kPa·s) ,2 0kV恒压电泳 (2 5℃ )分离 ,检测波长 2 4 0nm。在 1 0 .4～93 .5mg/L ,和 1 0 3～ 92 .7mg L范围内 ,对两种内酯分别进行了定量分析。加样回收率穿心莲内酯为 1 0 2 % ,脱水穿心莲内酯为 1 0 2 %。     

高效毛细管区带电泳法分离人血清蛋白质的研究

 研究了高效毛细管区带电泳分离人血清蛋白质的电泳行为及实验条件 ,建立了分离血清蛋白质的高效毛细管区带电泳法。血清样品经硼酸缓冲液 (5 0 mmol/L,p H8.80 )稀释后 ,以 0 .1 mol/L硼酸缓冲液 (p H9.3 5 ,含4g/L PEG80 0 0 )为电泳介质 ,在 5 0 μm i.d.× 3 7cm弹性石英毛细管柱 (有效柱长为 3 2 cm)中进行电泳分离 ,以2 0 0 nm紫外波长检测。方法简便、快速、重复性好 ,1 2 min内便可完成对血清中蛋白质的电泳分离。     

毛细管电泳法同时测定复方苦参注射液中三种生物碱含量

应用毛细管电泳法测定了复方苦参注射液中苦参碱、氧化苦参碱、槐定碱的含量。毛细管电泳条件为 :未涂层石英毛细管 ( 5 7cm× 5 0 μm i.d.) ,分离电压为1 2 .5 k V,0 .2 mol/ L Tris- 40 mmol/ L磷酸二氢钠 ( p H5 .5 0 ) - 2 0 %异丙醇为缓冲液 ,检测波长 2 0 0 nm,氢溴酸东莨菪碱为内标。结果表明 ,该法简便、快速、准确 ,重现性好。     

磺基水杨酸修饰电极联吡啶钌电化学发光体系测定可待因的研究

基于磷酸可待因对联吡啶钌在该电极上的电化学及其发光行为的增敏作用,建立了一种直接测定磷酸可待因的电化学发光新方法。在最佳实验条件下,磷酸可待因在1.0×10-4～4.0×10-6mol/L和4.0×10-6～2.0×10-7mol/L与相对发光强度呈线性关系,检出限为1.0×10-7mol/L(S/N=3)。连续测定4.0×10-7mol/l磷酸可待因5次,发光强度的RSD为2.7%。方法用于模拟尿样中磷酸可待因的测定,结果满意。     

高效毛细管电泳法测定罂粟壳中生物碱的含量

采用高效毛细管电泳法测定罂粟壳中可待因、吗啡和罂粟碱的含量,结果表明可待因的加样回收率为９６．６１％,吗啡为９５．９０％,罂粟碱为９５．３７％。方法简便、准确、重现性好,可作为生物碱的质量控制方法。     

Studies of Active Ingredients in Cough Syrup by Capillary Zone Electrophoresis with Amperometric Detection

The present paper covers a simple, reliable and reproducible method, based on capillary zone elec-trophoresis (CZE) with amperometric detection(AD), for the separation and the determination of ephedrine hydrochloride, promethazine hydrochloride and codeine phosphate. Under the optimal conditions, the three analytes were base-line separated completely within 16 min. Good linear relationships between the peak heights and the concentrations of the three analytes were obtained with the correlation coefficients better than 0. 9993. The method was directly applied to the determination of the active ingredients in pharmaceutical preparations and the assay results were satisfactory.     

Simultaneous determination of codeine and chlorpheniramine in human plasma by capillary column gas chromatography

A specific and highly sensitive capillary column gas chromatographic method was developed for the simultaneous determination of codeine and chlorpheniramine in human plasma. The method involves a solvent extraction and analysis by capillary column gas chromatography on a cross-linked 50% phenylmethyl silicone fused-silica capillary column with flame thermionic detection. A 10% solution of n-butanol in toluene was used as extraction medium and pyrilamine was used as internal standard. Reproducibility, linearity of calibration curves and specificity were all satisfactory with both drugs. The plasma concentration of codeine and chlorpheniramine could be measured at levels down to 0.9 ng/ml as codeine phosphate and 0.4 ng/ml as chlorpheniramine maleate, respectively. The method was applied to plasma samples from normal volunteers, and was confirmed to be adequate for biopharmaceutical and pharmacokinetic studies.     

毛细管区带电泳法快速测定复方布洛芬片的有效成分

 研究了用毛细管区带电泳法快速测定复方布洛芬片中布洛芬和伪麻黄碱含量的方法。在０．０２５ｍｏｌ／Ｌ的磷酸盐缓冲液（ｐＨ８．１）中，上述两组分可在３ｍｉｎ内得以完全分离，用紫外检测器在２１０ｎｍ处检测，并以外标法定量。１１次测定含有９．５ｍｇ／Ｌ盐酸伪麻黄碱和６６．７ｍｇ／Ｌ布洛芬的试样溶液，相对标准偏差为２．９％（伪麻黄碱）和１．９％（布洛芬），回收率为１０３．１％（伪麻黄碱）和９７．６％（布洛芬）。应用毛细管区带电泳法测定复方布洛芬片剂的含量，所得结果与ＨＰＬＣ法一致。     

毛细管区带电泳法快速测定复方布洛芬片的有效成分

研究了用毛细管区带电泳法快速测定复方布洛芬片中布洛芬和伪麻黄碱含量的方法。在０．０２５ｍｏｌ／Ｌ的磷酸盐缓冲液（ｐＨ８．１）中，上述两组分可在３ｍｉｎ内得以完全分离，用紫外检测器在２１０ｎｍ处检测，并以外标法定量。１１次测定含有９．５ｍｇ／Ｌ盐酸伪麻黄碱和６６．７ｍｇ／Ｌ布洛芬的试样溶液，相对标准偏差为２．９％（伪麻黄碱）和１．９％（布洛芬），回收率为１０３．１％（伪麻黄碱）和９７．６％（布洛芬）。应用毛细管区带电泳法测定复方布洛芬片剂的含量，所得结果与ＨＰＬＣ法一致。     

用高效毛细管电泳测定二(2'-脱氧-2'-氟)嘧啶核糖核苷酸对蛇毒磷酸二酯酶的稳定性

本文报道用高效毛细管电泳测定蛇毒磷酸二酯酶催化的二(2'-脱氧-2'-氟)嘧啶核糖核苷酸的水解速度。高效毛细管电泳用于这个目的有分辨率高、样品需要量'、使用不含有机溶剂的缓冲液和操作方便等优点。用来测定具有中等反应速度的反应是很方便的。     

Simultaneous high-performance liquid chromatographic stability-indicating analysis of acetaminophen and codeine phosphate in tablets and capsules

A high-performance liquid chromatographic method has been developed for the simultaneous determination of acetaminophen and codeine phosphate for product stability studies, and release and dissolution testing of tablets and capsules. The reversed-phase method utilizes UV detection at 214 nm, a C18 column and requires a maximum of 10 min per analysis. The method has been validated for use with products containing as much as 500 mg of acetaminophen and as little as 7.5 mg of codeine phosphate. The known potential degradation products, p-aminophenol, codeine N-oxide, and codeinone are separated for quantitation simultaneous with the parent compounds. The method has been shown to be linear, reproducible, specific, sensitive and rugged.     

Determination of ephedrine and codeine in human urine by cation-selective exhaustive injection and sweeping micellar electrokinetic chromatography

A sensitive method for the determination of ephedrine and codeine in human urine by capillary electrophoresis(CE)was described.In order to improve the sensitivity,two online concentration techniques including cation-selective exhaustive injection (CSEI)and sweeping micellar electrokinetic chromatography(sweeping-MEKC)were used.Under the optimum conditions,the detection limits(S/N=3)were 0.10μg/L for ephedrine and 0.80μg/L for codeine.This method was successfully applied to real urine sample analysis.     

Determination of phosphate in natural waters by capillary electrophoresis Influence of solution composition on migration time and response

This paper deals with the determination of the more complex phosphate anion by capillary electrophoresis using indirect UV detection. First, the pH of the running electrolyte influences both the migration time and the response of the phosphate anion. Both effects could be explained well by taking into account phosphorus speciation in solution. In addition, the experimental method has been applied to three different sets of natural water systems; (i) groundwater, (ii) surface water and (iii) stemflow samples. The migration time behaviour of phosphate was different for the three sample sets and, hence, difficulties arise with respect to a clear and unique identification of the compound. Deviations herein could be minimized by applying a correction method for migration time drift. Concentrations of phosphate could be quantified in most samples and were confirmed by a calorimetric method. Average recoveries of additions of phosphate to groundwater, surface water and stemflow samples were 105, 83 and 103%, respectively. For one stemflow sample, quantitative recovery of phosphate was possible only by changing the pH of the running electrolyte solution. The latter observation might be very useful in setting up speciation-related measurement methods.     

Separation of 2-aminobenzoic acid-derivatized glycosaminoglycans and asparagine-linked glycans by capillary electrophoresis.

A capillary electrophoresis method was developed for the analysis of oligosaccharides combined with derivatization with 2-aminobenzoic acid. Glycosaminoglycan delta-disaccharides were effectively resolved on a fused-silica capillary tube using 150 mM borate, pH 8.5, as a running electrolyte solution. This analytical method was applied to the identification of glycosaminoglycan in combination with enzymatic digestion. The separation of N-glycans or glucose-oligomers was performed with a phosphate buffer containing polyethylene glycol or borate as an electrolyte solution. This method is expected to be useful in the determination of oligosaccharide structures in a glycoprotein.     

毛细管区带电泳定量分析机体组织中高能磷酸化合物

研究了机体组织中三磷酸腺苷、二磷酸腺苷、一磷酸腺苷及磷酸肌酸的毛细管区带电泳分离条件;１２ｍｉｎ内完成上述４组分分离;其检出限分别为 ３．５、３．６、２．４、５．１ｍｇ／Ｌ;迁移时间及校正峰面积的定量精度分别低于０．１７％和３．８％。方法已用于猫心肌中上述４组分的定量分析。