Stability-Indicating HPTLC Method for Simultaneous Estimation of Amlodipine Besylate,Hydrochlorothiazide and Olmesartan Medoxomil in Combined Tablet Dosage Forms

JPC – Journal of Planar Chromatography – Modern TLC -     

流动注射-化学发光法测定苯磺酸氨氯地平

报道了基于铁氰化钾与鲁米诺化学反应,并应用IFFM-E型流动注射化学发光分析仪测定苯磺酸氨氯地平(ALDP)的方法。在碱性溶液中,上述化学发光反应的化学发光强度因ALDP的存在而显著增加,且其强度的增加值(△I)与ALDP的质量浓度分别在以下3个浓度区间呈线性关系:3.0×10~(-5)～8.0×10~(-5)g·L~(-1),8.0×10~(-5)～7.0×10~(-4)g·L~(-1)及7.0×10~(-4)～5.0×10~(-3)g·L~(-1)。方法的检出限(3σ)为8.5×10~(-7)g·L~(-1)。分析时取ALDP药片10片研碎为粉末状,称取其总质量的1/10溶于水中,定容至50mL,分取适量并稀释后供分析用。试样的进样体积为150μL,引入仪器的铁氰化钾溶液、氢氧化钠溶液及鲁米诺溶液的浓度依次为2.0×10~(-4),5.0×10~(-2),2.0×10~(-5)mol·L~(-1)。在已知ALDP含量的试样溶液中分别加入3个不同浓度的ALDP标准溶液,按方法测定后求得其回收率在96.0%～102.4%之间。对为5.0×10~(-4)g·L~(-1)ALDP标准溶液重复测定11次,所得相对标...     

Development of an Ion-Pair HPLC Method for Determination of Acebutolol in Pharmaceuticals

A simple and accurate ion-pair reversed-phase high-performance liquid chromatographic (RP-HPLC) method has been developed and validated for determination of acebutolol (ACE) in tablet dosage forms. Both ACE and ambroxol (internal standard) were well separated using a reversed phase column and a mobile phase consisting of a mixture of methanol-0.05 M acetic acid (containing 8 mM sodium 1-heptanesulfanate) (65:35 v/v) with pH adjusted to 3.2 with triethylamine. The mobile phase was pumped at 0.80 mL min^?1 flow rate and ACE was detected by diode-array detection at 240 nm. The retention times for ACE and internal standard (IS) were 4.574 and 8.236 min, respectively. A linear response (r = 0.9998) was observed in the range of 0.27–2.93 μg mL^?1 in mobile phase. The limit of detection and limit of quantification were found as 0.07 and 0.23 μg mL^?1 in the mobile phase. Validation parameters such as precision, accuracy, selectivity, reproducibility, and system suitability tests were also determined. The excipients did not interfere with the assay of ACE in tablet dosage forms. It is suggested that the proposed method can be used for routine quality control and dosage-form assay of ACE.     

Simultaneous Enantioseparation and Rapid Determination of Atenolol and Amlodipine Besylate by Capillary Electrochromatography

Chromatographia - Simultaneous enantioseparation and rapid determination method of atenolol (AN) and amlodipine besylate (AMB) was firstly established using diphenylmethane...     

A Validated RP–LC Method for Simultaneous Determination of Losartan Potassium and Amlodipine Besilate in Pharmaceutical Preparations

A simple RP–LC method for simultaneous quantification of losartan and amlodipine and separation of their degradation products has been developed. For this purpose we tested appropriated mobile phase pH range, flow rate, temperature and different columns. The method was validated with an ODS column. A gradient of acetonitrile and phosphate pH 3.0 buffer was utilized as mobile phase. The linearity was determined at 50–150% level. Individual recoveries at 70–130% level ranged from 98.8 to 100.5% for losartan and 96.4–101.2% for amlodipine. The robustness was also evaluated. Although losartan has much higher quantities than amlodipine in commercial tablets, this method allowed simultaneous quantification for both drugs.     

A Validated RP–LC Method for Simultaneous Determination of Losartan Potassium and Amlodipine Besilate in Pharmaceutical Preparations

A simple RP–LC method for simultaneous quantification of losartan and amlodipine and separation of their degradation products has been developed. For this purpose we tested appropriated mobile phase pH range, flow rate, temperature and different columns. The method was validated with an ODS column. A gradient of acetonitrile and phosphate pH 3.0 buffer was utilized as mobile phase. The linearity was determined at 50–150% level. Individual recoveries at 70–130% level ranged from 98.8 to 100.5% for losartan and 96.4–101.2% for amlodipine. The robustness was also evaluated. Although losartan has much higher quantities than amlodipine in commercial tablets, this method allowed simultaneous quantification for both drugs.     

Validated HPLC and HPTLC Method for Simultaneous Quantitation of Amlodipine Besylate and Olmesartan Medoxomil in Bulk Drug and Formulation

Two methods are described for simultaneous determination of amlodipine besylate and olmesartan medoxomil in formulation. The first method was based on the HPTLC separation of two drugs on Merck HPTLC aluminium sheets of silica gel 60 F₂₅₄ using n-butanol: acetic acid: water (5:1:0.1, v/v/v) as the mobile phase. The second method was based on the HPLC separation of the two drugs on the RP-PerfectSil-100 ODS-3–C₁₈ column from MZ-Analysetechnik GmbH, Germany and acetonitrile/0.03 M ammonium acetate buffer (pH = 3) in a ratio of 55:45 as the mobile phase. Both methods have been applied to formulation without interference of excipients of formulation.     

Simultaneous Determination of Hydrochlorothiazide and Reserpine in Human Urine by LC with a Simple Pre-Treatment

A simple, selective and sensitive reversed-phase high performance liquid chromatography method for simultaneous analysis of hydrochlorothiazide and reserpine in human urine was developed and subjected to primary pharmacokinetic study. After a simple protein precipitation using methanol and extraction with ethyl acetate, the analytes were separated on an Elite C(18) column at a flow rate of 0.8 mL min(-1). The mobile phase was composed of acetonitrile (A) and 0.2% ammonium chloride solution (B) for a gradient elution starting at A:B at 30:70, v/v for 0~6 min, linearly raising the percent of A from 30% to 50% (6~9 min) and ending at 50:50, v/v (9~25 min). The standard curves were linear over the range of 0.05-20 μg mL(-1) for hydrochlorothiazide and 0.02-5.0 μg mL(-1) for reserpine, respectively (r > 0.999). The limit of detection (LOD) and the limit of quantification (LOQ) were 5.5 ng mL(-1) and 18.2 ng mL(-1) for hydrochlorothiazide, and 7.1 ng mL(-1) and 23.6 ng mL(-1) for reserpine, respectively. The recoveries for both analytes were above 89.0±1.35%. The intra-day and inter-day precision for hydrochlorothiazide were less than 1.91% and 1.38%, and those for reserpine were below 1.61% and 2.64%, respectively. The method indicated good performance in terms of specificity, linearity, detection and quantification limits, precision and accuracy, and it was employed successfully for the simultaneous determination of hydrochlorothiazide and reserpine in human urine samples.     

A Partial Least-Squares Multivariate Calibration Method for the Simultaneous Spectrophotometric Determination of Spironolactone,Canrenone and Hydrochlorothiazide

Abstract

An application of a partial least squares calibration method for the simultaneous spectrophotometric determination of spironolactone, canrenone and hydrochlorothiazide is suggested. The use of the PLS for the multicomponent spectrophotometric determination is demonstrated on the analysis of several synthetic mixtures. It was shown that is possible to resolve complex mixtures of     

时间分辨-后化学发光法同时测定阿米卡星和氢氯噻嗪

根据阿米卡星、氢氯噻嗪在过氧化单硫酸盐(PMS)-鲁米诺(Luminol)体系中的化学发光反应的动力学性质有着明显的差异性,建立了同时测定阿米卡星和氢氯噻嗪新的时间分辨后化学发光的方法。在PMS-鲁米诺体系中,氢氯噻嗪化学发光反应较快,1 s达到最大值,峰尖锐;而阿米卡星化学发光反应较慢,37.9 s后达到最大值,峰平缓,且其动力学曲线呈现出随时间分开的两个独立的发光峰,互不干扰。结果表明;氢氯噻嗪和阿米卡星的线性范围分别为8.0×10-5～4.0×10-3g/L和8.0×10-4～4.0×10-2g/L;11次平行测定4.0×10-4g/L氢氯噻嗪溶液和4.0×10-3g/L阿米卡星溶液的化学发光强度相对标准偏差分别为2.4%和3.7%。本方法测定氢氯噻嗪和阿米卡星的检出限分别为2.0×10-5和2.0×10-4g/L。     

Simultaneous Spectrophotometric Determination of Hydrochlorothiazide and Pharmaceutical Preparations

Abstract

We developed three methods for the simultaneous determination of amiloride (AMI) and hydrochlorothiazide (HCT): zero-crossing, derivative quotient spectra with normalized divisor and multiple linear regression (MULTIC) methods. The two first methods use the derivative spectrophotometry, and the last one uses the absorbance measurement. The three methods were used to determine both compounds in synthetic mixtures and pharmaceutical preparations with errors less than 5% and 15%, respectively.     

Simultaneous LC–MS–MS Analysis of Valsartan and Hydrochlorothiazide in Human Plasma

A rapid and specific liquid chromatographic–tandem mass spectrometric method is described for simultaneous analysis of valsartan (VAL) and hydrochlorothiazide (HCTZ) in human plasma. VAL and HCTZ were chromatographed on a C₈ column with 75:15:10 (v/v) acetonitrile–methanol–0.001% aqueous ammonia as mobile phase. VAL and HCTZ were eluted at 0.69 min and 1.22 min, respectively, and, after electrospray ionization (ESI), detected in selected-reaction-monitoring mode. The precursor to product-ion transitions m/z 434.32 → 179.22 and m/z 295.85 → 204.86 were used to quantify VAL and HCTZ, respectively. Recovery by solid-phase extraction was >90% for both analytes and the internal standard. The method was suitable for application to a pharmacokinetic study after oral administration of tablet containing 160 mg VAL and 25 mg HCTZ to 18 healthy volunteers.     

Oil-In-Water Microemulsion LC Determination of Pharmaceuticals Using Gradient Elution

Efficient and novel oil-in-water microemulsion HPLC (MELC) separations of a range of solutes have been performed on conventional reversed-phase HPLC columns using gradient elution. This work follows previous successful separations using isocratic oil-in-water MELC [1]. It was found that by changing certain variables, peak-peak resolution, separation selectivity, efficiency and solute retention could be manipulated. The method was compatible with very low UV detection wavelengths. A robust separation method was developed for the quantitative analysis of 2 steroids in a combination-inhaled product for asthma. The method offered similar chromatography and run time when compared with conventional HPLC modes, thus demonstrating its potential for routine use. Stability-indicating methods were developed to separate synthetic and degradative impurities from the main component peaks in 4 pharmaceutical products. The methods offered quicker analysis times and equivalent selectivity to conventional HPLC modes. In developing the separations the effect on the chromatography of varying the operating parameters was studied.     

Simultaneous RP-LC Determination of Losartan Potassium, Ramipril, and Hydrochlorothiazide in Pharmaceutical Preparations

A simple, rapid, and precise reversed-phase high-performance liquid chromatographic method has been developed for simultaneous determination of losartan potassium, ramipril, and hydrochlorothiazide. The three drugs were separated on a 150 mm × 4.6 mm i.d., 5 μm particle, Cosmosil C₁₈ column. The mobile phase was 0.025 m sodium perchlorate–acetonitrile, 62:38 (v/v), containing 0.1% heptanesulphonic acid, pH adjusted to 2.85 with orthophosphoric acid, at a flow rate of 1.0 mL min⁻¹. UV detection was performed at 215 nm. The method was validated for linearity, accuracy, precision, and limit of quantitation. Linearity, accuracy, and precision were acceptable in the ranges 35–65 μg mL⁻¹ for losartan, 1.75–3.25 μg mL⁻¹ for ramipril, and 8.75–16.25 μg mL⁻¹ for hydrochlorothiazide.     

A Novel Potentiometric Detection Strategy for the Determination of Amlodipine Besylate Based on Functionalized Particles

A novel potentiometric strategy based on functionalized magnetite nanoparticles and microparticles were compared with the classical potentiometric strategy. This strategy provided nano‐ and microsized particles that were highly dispersed and coated with ionophore and plasticizer to promote an in situ cooperative ion‐pairing interaction between the ionophore and the analyte present in inner solution of sensor membrane, compared to the classical technique. Three amlodipine (AML) sensors were constructed using functionalized nanoparticles in sensor 1; microparticles in sensor 2, as ionophores, and the polymeric membrane ionophoric property in sensor 3.     

A Stability-Indicating LC Method for the Simultaneous Determination of Telmisartan and Ramipril in Dosage Form

A simple, rapid, and precise method is developed for the quantitative simultaneous estimation of telmisartan and ramipril in combined pharmaceutical dosage form. A chromatographic separation of the two drugs was achieved with an ACE 5 C₁₈, 25-cm analytical column using buffer–acetonitrile (55:45 v/v). The buffer used in mobile phase contains 0.1 M sodium perchlorate monohydrate in double distilled water pH adjusted 3.0 with trifluoroacetic acid. The instrumental settings are flow rate of 1.5 mL min⁻¹, column temperature at 30 °C, and detector wavelength of 215 nm using a photodiode array detector. The resolution between ramipril and telmisartan were found to be more than 5. Theoretical plates for ramipril and telmisartan were 13,022 and 6,629. Tailing factor for ramipril and telmisartan was 0.94 and 0.98. Telmisartan, ramipril and their combination drug product were exposed to thermal, photolytic, hydrolytic and oxidative stress conditions, and the stressed samples were analysed by the proposed method. Peak homogeneity data of telmisartan and ramipril is obtained using photodiode array detector, in the stressed sample chromatograms, demonstrated the specificity of the method for their estimation in presence of degradants. The described method shows excellent linearity over a range of 20–400 μg mL⁻¹ for telmisartan and 2.5–50 μg mL⁻¹ for ramipril. The correlation coefficient for telmisartan and ramipril are 1. The relative standard deviation for six measurements in two sets of each drug in tablets was always less than 2%. The proposed method was found to be suitable and accurate for quantitative determination and the stability study of telmisartan and ramipril in pharmaceutical preparations.     

A Validated LC Method for Simultaneous Determination of Three Major Components in Entada phaseoloides

A high performance liquid chromatography method was developed for the simultaneous determination of three major active constituents in Entada phaseoloides, namely phaseoloidin (1), entadamide A (2), entadamide A-β-d-glucopyranoside (3), respectively. The samples were separated on an Aglient Eclipse XDB-C₁₈ column with gradient elution of acetonitrile and 0.3% phosphoric acid (v/v) at a flow rate of 1.0 mL min^?1 and detected at 280 nm. The three target compounds were completely separated within 10 min. All calibration curves showed good linearity (r > 0.9999) within test ranges. The reproducibility was evaluated by intra- and inter-day assays and RSD values were less than 1.04%. The recoveries were between 97.15 and 101.95%. The method was successfully applied to the analysis of three compounds in 22 commercial samples of E. phaseoloides. The results indicated that the developed LC assay was readily utilized as a quality control method for E. phaseoloides.     

Electroanalytical Studies and Simultaneous Determination of Amlodipine Besylate and Atorvastatine Calcium in Binary Mixtures Using First Derivative of the Ratio‐Voltammetric Methods

The electrochemical behavior of atorvastatin and amlodipine at a glassy carbon electrode has been studied using different voltammetric techniques. First derivative of the ratio voltammetric methods for determination of amlodipine and atorvastatin in tablets in the presence of the other compound has been described. This technique depends on the measuring of first derivative of the ratio voltammograms of each concentration as a function of the increased concentrations. DP and SW voltammetric methods depend on first derivative of the ratio‐voltammetry by measurements of the selected potentials for amlodipine and atorvastatin. The linear response was within the range of 4×10^?6–1×10^?4 M for amlodipine and 2×10^?6–1×10^?4 M for atorvastatin. The proposed methods have been extensively validated.     

Simultaneous Determination of Cilazapril and Hydrochlorothiazide in Tablets by Spectrophotometric Methods

Abstract

In this study, two new spectrophotometric methods were used for the simultaneous determination of cilazapril and hydrochlorothiazide in their binary mixture. In the first method, derivative spectrophotometry, dA/dδ values were measured at 242.8 nm and 282.8 nm for cilazapril and hydrochlorothiazide, respectively, in the first derivative spectra of their combination. The relative standard deviation of the method was found to be 0.77% for cilazapril and 0.24% for hydrochlorothiazide. In the second, the absorbancy ratio method, the quantification of cilazapril and hydrochlorothiazide was performed by using the absorbances read at 210.4 nm. 250.2 nm and 270.6 nm in the zero-order spectra of their mixture; relative standard deviations of the method were found to be 1.26 % and 0.81 % for cilazapril and hydrochlorothiazide, respectively. These two methods have been successfully applied to a tablet containing these drugs.