Simultaneous determination of phenylephrine hydrochloride, guaifenesin, and chlorpheniramine maleate in cough syrup by gradient liquid chromatography

A simple and reliable high-performance liquid chromatographic method was developed for the simultaneous determination of mixture of phenylephrine hydrochloride (PHENYL), guaifenesin (GUAIF), and chlorpheniramine maleate (CHLO) either in pure form or in the presence of methylparaben and propylparaben in a commercial cough syrup dosage form. Separation was achieved on a C8 column using 0.005 M heptane sulfonic acid sodium salt (pH 3.4 +/- 0.1) and acetonitrile as a mobile phase by gradient elution at different flow rates, and detection was done spectrophotometrically at 210 nm. A linear relationship in the range of 30-180, 120-1800, and 10-60 microg/mL was obtained for PHENYL, GUAIF, and CHLO, respectively. The results were statistically analyzed and compared with those obtained by applying the British Pharmacopoeia (2002) method and showed that the proposed method is precise, accurate, and can be easily applied for the determination of the drugs under investigation in pure form and in cough syrup formulations.     

Simultaneous spectrophotometric and liquid chromatographic determination of dextromethorphan hydrobromide,phenylephrine hydrochloride,and carbinoxamine maleate in pharmaceutical preparations

Simultaneous determination of dextromethorphan hydrobromide (DEX), phenylephrine hydrochloride (PHEN), and carbinoxamine maleate (CAR) in pharmaceutical preparations was performed by using liquid chromatograpy (LC) and spectrophotometry. In LC, the separation was achieved on a C18 column and the optimal mobile phase for satisfactory separation in a gradient elution program was found to be acetonitrile-sodium perchlorate solution (5: 95, v/v) initially, then a linear gradient up to 60% acetonitrile in 8 min. In spectrophotometric method, a chemometric technique, principal component regression (PCR), was used. In the method, the absorbance data matrix corresponding to the concentration data matrix was obtained by the measurement of absorbances in their zero order spectra by Δλ = 1 nm in the 210–300 nm range. Then, the calibration was obtained by using this data matrix for the prediction of unknown concentrations of DEX, PHEN, and CAR in their ternary mixture. The methods proposed were validated and successfully applied to a pharmaceutical preparation, capsule, and the results were compared.     

High-pressure liquid chromatographic assay of dextromethorphan hydrobromide, guaifenesin, and sodium benzoate in an expectorant syrup

An ion-pair reversed-phase high-pressure liquid chromatographic assay is developed that allows simultaneous quantitation of guaifenesin, dextromethorphan hydrobromide, and sodium benzoate in an expectorant syrup. The method is rapid and accurate. Average recoveries of 99.6, 99.8, and 99.7% with relative standard deviations of 0.5, 0.9, and 0.2% are obtained for guaifenesin, dextromethorphan hydrobromide, and sodium benzoate, respectively, from laboratory prepared samples. Chromatographic conditions are selected to afford a pH that provides adequate separation of guaifenesin, dextromethorphan hydrobromide, sodium benzoate, and sodium saccharin and a detection wavelength that effectively compensates for the great disparity in quantity between guaifenesin and dextromethorphan hydrobromide present in syrups. The relationships between the retention volume of dextromethorphan hydrobromide and the alkyl chain length as well as the concentration of the counterion are studied. The retention profiles for sodium saccharin, guaifenesin, sodium benzoate, and dextromethorphan hydrobromide in the apparent pH range of 2.5 to 6.6 are established.     

Assay of mixtures of chlorpheniramine maleate,pyrilamine meleate and phenylpropanolamine hydrochloride in cold-allergy tablets by difference spectrophotometry

Mixtures of chlorpheniramine maleate (CPM) and phenylpropanolamine hydrochloride (PPA), with and without pyrilamine maleate (PRM), are assayed by u.v. difference spectrophotometry without prior separation. The spectra for CPM and PRM in solutions at pH 1 and pH 6 show differences whereas the spectra for PPA remain the same at pH 1 and 6. For PPA, quantitation is based on the spectral change on oxidation to benzaldehyde with metaperiodate; this oxidation does not affect CPM and PRM. Calibration plots are linear for 6.7–99.9 μg ml^?1 CPM (r = 0.9992), 12.7–50.6 μg ml^?1 PRM (r = 0.9997) and 25–115.3 μg ml^?1 PPA (r = 0.9980) in the presence of one another. Average recoveries (± RSD) from simulated PPA/CPM tablets were: PPA, 98.4 ± 0.4% (without PRM, n = 3), 99.8 ± 0.4% (with PRM, n = 5); CPM, 99.3 ± 0.6% (without PRM, n = 3), 99.2 ± 0.4% (with PRM, n = 5); and PRM, 99.5 ± 0.2% (in PPA/CPM/PRM tablets, n = 5). The method was successfully applied to commercial cold-allergy tablets containing these compounds.     

Simultaneous determination of pseudoephdrine, pheniramine, guaifenisin, pyrilamine, chlorpheniramine and dextromethorphan in cough and cold medicines by high performance liquid chromatography

A new simple, rapid and sensitive liquid chromatographic method has been developed and validated for the simultaneous determination of pseudoephdrine, pheniramine, guaifenisin, pyrilamine, chlorpheniramine and dextromethorphan in cough and cold pharmaceuticals. The separation of these compounds was achieved within 13 min on a Kromasil C18 column using an isocratic mobile phase consisting of methanol-dihydrogenphosphate buffer at pH 3 (45:55, v/v). The analysis was performed at a flow rate of 1 mL min⁻¹ and at a detection wavelength of 220 nm. The selectivity, linearity of calibration, accuracy, within and between-days precision and recovery were examined as parts of the method validation. The concentration-response relationship was linear over a concentration range of 5-50 μg mL⁻¹ for pseudoephdrine, pheniramine, chlorpheniramine and 50-600 μg mL⁻¹ for guaifenisin, pyrilamine, dextromethorphan, methylparaben and sodium benzoate with correlation coefficients better than 0.998. The standard deviations of the intraday and interday were all less than 2%. The proposed liquid chromatographic method was successfully applied for the routine analysis of these compounds in different cough and cold pharmaceutical preparations such as syrups, capsules, tablets and sachets. The presence of preservatives (sodium benzoate and methylparaben) and other excipients did not show any significant interference on the determination of these compounds.     

Experimental design of reversed-phase high performance liquid chromatographic conditions for simultaneous determination of ibuprofen,pseudoephedrine hydrochloride,chlorpheniramine maleate,and nipagen

2^5-1 fractional factorial design was applied to optimize the chromatographic conditions of the RP-HPLC determination of ibuprofen, pseudoephedrine hydrochloride, chlorpheniramine maleate, and nipagen in syrup preparation. All the factors that affect the determination of components and their interactions were investigated. pH, flow rate and solvent ratios for three steps of gradient profile were regarded as factors to be investigated in two levels. The resolution was chosen as analytical response. The limit of quantitations (10 s/m) were found as 0.9, 1.0, 0.4, and 0.12 μg/mL for ibuprofen, pseudoephedrine hydrochloride, chlorpheniramine maleate, and nipagen, respectively.     

Simultaneous determination of paracetamol,phenylephrine hydrochloride and chlorpheniramine maleate in pharmaceutical preparations using multivariate calibration 1

Resolution of binary mixtures of paracetamol, phenylephrine hydrochloride and chlorpheniramine maleate with minimum sample pre-treatment and without analyte separation has been successfully achieved by methods of partial least squares algorithm with one dependent variable, principal component regression and hybrid linear analysis. Data of analysis were obtained from UV–vis spectra of the above compounds. The method of central composite design was used in the ranges of 1–15 mg L^?1 for both calibration and validation sets. The models refinement procedure and their validation were performed by cross-validation. Figures of merit such as selectivity, sensitivity, analytical sensitivity and limit of detection were determined for all three compounds. The procedure was successfully applied to simultaneous determination of the above compounds in pharmaceutical tablets.     

Development and validation of chemometrics-assisted spectrophotometry and liquid chromatography methods for the simultaneous determination of the active ingredients in two multicomponent mixtures containing chlorpheniramine maleate and phenylpropanolamine hydrochloride

Multivariate spectrophotometric calibration and liquid chromatography (LC) methods were used for the simultaneous determination of the active ingredients in 2 multicomponent mixtures containing chlorpheniramine maleate and phenylpropanolamine hydrochloride with ibuprofen and caffeine (mixture 1) or with propyphenazone (mixture 2). For the multivariate spectrophotometric calibration methods, principal component regression (PCR) and partial least squares (PLS-1), a calibration set of the mixtures consisting of the components of each mixture was prepared in distilled water. A leave-1-out cross-validation procedure was used to find the optimum numbers of latent variables. Analytical parameters such as sensitivity, selectivity, analytical sensitivity, limit of quantitation, and limit of detection were determined for both PLS-1 and PCR. The LC method depends on the use of a cyanopropyl column with the mobile phase acetonitrile-12 mM ammonium acetate, pH 5.0 (25 + 75, v/v), for mixture 1 or acetonitrile-10 mM potassium dihydrogen phosphate, pH 4.7 (45 + 55, v/v), for mixture 2; the UV detector was set at 212 nm. In spite of the presence of a high degree of spectral overlap of these components, they were rapidly and simultaneously determined with high accuracy and precision, with no interference from the matrix excipients. The proposed methods were successfully applied to the analysis of pharmaceutical formulations and laboratory-prepared mixtures containing the 2 multicomponent combinations.     

反相高效液相色谱法同时测定对苯氧基苯酚和对氯苯酚

建立了一种同时测定对苯氧基苯酚和对氯苯酚的反相高效液相色谱方法。采用Diamonsil(钻石)C18(250 mm×4.6 mm i.d.,5μm)色谱柱,以甲醇-水(V(甲醇):V(水)=8∶2)为流动相,在波长为230 nm处进行检测。对苯氧基苯酚和对氯苯酚在20~230μg/mL范围内,峰面积与质量浓度呈良好的线性关系,相对标准偏差RSD分别为0.26%、0.53%,回收率在99.0%~101%之间。方法可用于对苯氧基苯酚的合成工艺研究及成品质量控制。     

Separation of isomeric and nonisomeric monoribonucleotides by isocratic ion pair high performance liquid chromatography

A simple, isocratic, high performance liquid chromatographic procedure is described for the first time for the separation of nine monoribonucleotides using the ion-pairing technique. An aqueous mobile phase containing 100 mM KH₂PO₄ and 12.5 mM tetramethylammonium hydroxide as the solvophobic ion, pH 3.9, was used with a reverse phase RP-18 column. The nine monoribonucleotides studied were separated and eluted in the following order: cytidine-5′ -phosphate, uridine-5′ -phosphate, cytidine-3′ -phosphate, guanosine-5′ -phosphate, uridine-3′ -phosphate, uridine-2′ -phosphate, adenosine-5′ -phosphate, guanosine-3′ -phosphate, and adenosine-3′ -phosphate. Generally the 5′ nucleotides eluted faster than the 3′ and the order of elution within each series was: cytidine, uridine, guanosine, and adenosine. The only nucleotide where three isomers were studied was uridine, and the 2′ eluted later than the 3′. Baseline separation was attained for a mixture containing four 3′ nucleotides and uridine-2′ -phosphate. When the four 5′ nucleotides were chromatographed, baseline separation was also obtained except between cytidine-5′ -phosphate and uridine-5′ -phosphate. The coefficient of variation of the retention characteristics, which reflected day-to-day variation, averaged 6.4%.     

Simultaneous high-performance liquid chromatographic determination of paracetamol, phenylephrine HCl, and chlorpheniramine maleate in pharmaceutical dosage forms

A rapid, precise, and specific high-performance liquid chromatographic method is described for the simultaneous determination of paracetamol, phenylephrine HCI, and chlorpheniramine maleate in combined pharmaceutical dosage forms. The method involves the use of a microBondapak CN RP analytical column (125 A, 10 microm, 3.9 x 150 mm) at 22 degrees C as the stationary phase with the mixture of acetonitrile and phosphate buffer (pH 6.22, 78:22) as the mobile phase. Derivatization of the drugs is not required. The method is applied to commercial pediatric cough-cold syrups, tablets, and capsules marketed in Turkey. The relative standard deviation for 10 replicate measurements of each drug in the medicaments is always less than 2%.     

Application of ion pair high performance liquid chromatography to the analysis of porphyrins in clinical samples

Reversed phase ion pair chromatography is a highly selective separation technique for the determination of free porphyrin carboxylic acids from human materials. Isocratic and gradient elution methods can be used to analyse porphyrin isomers and to establish porphyrin profiles for the biochemical diagnosis of porphyrias. Ion pair high performance liquid chromatography led to the discovery of the atypical isomers II and IV of uroporphyrin and coproporphyrin in human urine. Advantages and limitations of the ion pair technique are discussed.     

Thermodynamics of the sorption of water-soluble vitamins in reverse-phase high performance liquid chromatography

The thermodynamics of the sorption of certain water-soluble vitamins on a C18 reverse phase from water-acetonitrile solutions of different compositions is studied. The thermodynamic characteristics of the investigated chromatographic systems are calculated. The dependences of standard molar enthalpy and changes in entropy when the sorbate transfers from the bulk solution to the surface layer on the concentration of the organic component in the mobile phase are analyzed. The boundaries for applying the main retention models describing the sorption of the investigated compounds are discussed.     

复合维生素片剂中泛酸钙的反相高效液相色谱法测定

用十八烷基硅烷键合硅胶为填充剂,以V（水）：V（甲醇）：V（H3PO4）=950：50：1为流动相,检测波长为210 nm,采用反相高效液相色谱法分离测定了两种复合维生素片剂中的泛酸钙,实验回收率在99.2%～103.4%之间,相对标准偏差RSD为0.6%～1.0%（n=5）,检出限为41 ng.已用于复合维生素片剂中泛酸钙的测定.     

反相高效液相色谱法测定化妆品中辅酶Q10的含量

建立一种测定化妆品中辅酶Q10含量的反相高效液相色谱方法.样品用异丙醇振荡萃取后,经C18固相萃取小柱净化.以Hypersil ODS2(5 μm,150 mm×4.6 mm i.d)作分析柱,以辅酶Q9为内标,异丙醇-甲醇(V(异丙醇)V(甲醇)=23)作流动相,在波长275 nm处进行检测.在0.5～100mg/L范围内,峰高比与质量浓度比呈良好的线性关系,化妆品中辅酶Q1o的检出限为0.76ng.方法的RSD《5%.     

Determination of phenylephrine hydrochloride, chlorpheniramine maleate, and methscopolamine nitrate in tablets or capsules by liquid chromatography with two UV absorbance detectors in series

A procedure is presented for the simultaneous determination of phenylephrine HCI (PE), chlorpheniramine maleate (CM), and methscopolamine nitrate in commercial tablets or capsules by liquid chromatography (LC) with 2 UV absorbance detectors in series. Reference and sample solutions are prepared in methanol. LC separations are performed on a 7.5 cm Novapak silica column. The mobile phase is prepared by mixing 930 mL methanol with 70 mL of a 0.5% aqueous solution of 1-pentanesulfonic acid, sodium salt. The injection volume is 20 microL; the flow rate is approximately 1 mL/min. Retention times are approximately 1.5 min for PE, 3 min for CM, and 6 min for methscopolamine nitrate. One detector determines the first 2 compounds at 265 nm, but the third compound does not produce a detectable peak. The other detector set at 210 nm generates peaks for all 3 compounds, but only methscopolamine is within the recorder range; the other 2 compounds are exceedingly off scale. If it is not feasible or desirable to arrange 2 UV absorbance detectors in series, separate determinations can be made, one for the first 2 compounds and the other for the third component of the mixture. Two commercial samples of tablets and 2 commercial samples of capsules were analyzed by the proposed method. Recovery studies were also conducted with amounts of the 3 compounds ranging from 80 to 120% of the quantities present in the sample solutions.     

Chromatographic performance of deuterated solvents in reversed phase micro high performance liquid chromatography

The chromatographic performance of the deuterated solvents, CD₃OD and D₂O, has been investigated in reversed-phase micro high performance liquid chromatography. The chromatographic performance of CD₃OD is only slightly superior to that of CH₃OH. However, the performance of D₂ is significantly superior to that of H₂O, separation of aromatics being improved by about 30%. D₂ is a particularly powerful solvent for the separation iof deuterated and non-deuterated compounds.     

Simultaneous determination of chlorpheniramine maleate and dexamethasone in a tablet dosage form by liquid chromatography

An accurate, simple, reproducible, and sensible liquid chromatographic method was developed and validated for the determination of chlorpheniramine maleate and dexamethasone in a tablet formulation. The analysis was performed at room temperature on a reversed-phase C18 column with UV detection at 254 nm. The mobile phase consisted of 7.5 mM monobasic potassium phosphate in methanol-water (62.5 + 37.5) at a constant flow rate of 1 mL/min. The method was validated in terms of linearity, precision, accuracy, and specificity by forced decomposition of chlorpheniramine maleate and dexamethasone initiated by using acid, base, water, hydrogen peroxide, heat, and light. The response was linear in the ranges of 0.04-0.12 and 0.006-0.016 mg/mL for chlorpheniramine maleate (r2 = 0.9999) and dexamethasone (r2 = 0.9994), respectively. The relative standard deviation values for intra- and interday precision studies were 2.39 and 2.02, respectively, for chlorpheniramine maleate and 2.39 and 1.25, respectively, for dexamethasone. Recoveries ranged from 95.07 to 101.95% for chlorpheniramine maleate and from 97.75 to 102.10% for dexamethasone.