scholarly journals Quantitative analysis of Loperamide hydrochloride in the presence its acid degradation products

2009 ◽  
Vol 63 (1) ◽  
pp. 39-46 ◽  
Author(s):  
Ivana Savic ◽  
Goran Nikolic ◽  
Ivan Savic ◽  
Valentina Marinkovic
Keyword(s):  
Mobile Phase ◽  
Degradation Products ◽  
Rapid Determination ◽  
Parent Compound ◽  
Ammonium Hydroxide ◽  
High Sensitivity ◽  
Hplc Method ◽  
Pharmaceutical Formulation ◽  
Acid Degradation

The aim of this work was to develop a new RP-HPLC method for the determination of loperamide hydrochloride in the presence of its acid degradation products. Separation of loperamide from degradation products was performed using ZORBAX Eclipse XDB C-18, column with a mobile phase consisting of 0.1% sodium-octansulphonate, 0.05% triethylamine, 0.1% ammonium hydroxide in water:acetonitrile (45:55 v/v). The mobile phase was adjusted to pH 3.2 with phosphoric acid. The method showed high sensitivity with good linearity over the concentration range of 10 to 100 ?g cm-3. The method was successfully applied to the analysis of a pharmaceutical formulation (Loperamide, Zdravlje-Actavis, Serbia) containing loperamide hydrochloride with excellent recovery. The loperamide hydrochloride degradation during acid hydrolysis and kinetics investigation was carried out in hydrochloric acid solutions of 0.1, 1.0 and 1.5 mol dm-3, at different temperatures (25 and 40?C), by monitoring the parent compound itself. The first order reaction of loperamide degradation in acid solution was determined. The activation energy was estimated from the Arrhenius plot and it was found to be 38.81 kJ mol-1 at 40?C. The developed procedure was successfully applied for the rapid determination of loperamide hydrochloride in pharmaceutical formulation (Loperamide, Zdravlje-Actavis, Serbia) and in the presence of its acid degradation products.

scholarly journals A Validated RP-HPLC Method and Force Degradation Studies of Fexofenadine Hydrochloride in Pharmaceutical Dosage Form

2018 ◽  
Vol 17 (1) ◽  
pp. 43-50
Author(s):  
Sherejad Sanam ◽  
Sharmin Nahar ◽  
Nazmus Saqueeb ◽  
SM Abdur Rahman
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Parent Compound ◽  
Hplc Method ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Fexofenadine Hcl

A stability indicating HPLC method was developed and validated for the quantitative determination of fexofenadine hydrochloride. An isocratic separation was achieved using phenomenex (C18) column (250×4.6 mm, 5 μm) with flow rate of 1.0 ml/min and UV detection at 254 nm. The mobile phase consists of 5Mm acetate buffer: acetonitrile (50:50; v/v) with pH 9.4 adjusted with acetic acid. The drug was subjected to oxidative, acidic, basic, neutral, photolytic and thermal degradation. All degradation products were eluted in an overall analytical run time of approximately 40 min with the parent compound fexofenadine hydrochloride at a flow rate of approximately 3.3±0.3 min. The method was linear over the concentration range of 31.5-500 μg/ml (r2 = 0.999) with limit of detection and quantification of 3.5 μg/ml and 10.1 μg/ml, respectively. The method has the requisite accuracy, selective, precision and robustness to assay fexofenadine HCl in tablets.Dhaka Univ. J. Pharm. Sci. 17(1): 43-50, 2018 (June)

scholarly journals Photostability study of amlodipine besylate tablets packed in primary packaging

2021 ◽  
Vol 10 (1) ◽  
pp. 20-28
Author(s):  
Ivana Savić-Gajić ◽  
Ivan Savić ◽  
Predrag Sibinović ◽  
Valentina Marinković
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Hplc Method ◽  
Coefficient Of Determination ◽  
Amlodipine Besylate ◽  
Limit Of Quantification ◽  
First Order Kinetics ◽  
The Given

In this study, the modified stability-indicating RP-HPLC method was validated for quantitative analysis of amlodipine besylate in the presence of its impurity D (3-ethyl 5-methyl 2-[(2-aminoethoxy)methyl]-4-(2-chlorophenyl)-6-methylpyridine-3,5-dicarboxylate). The method was applied for the determination of an analyte in the tablets and irradiated samples packed in the primary packaging (Alu/PVC/PVDC blister packaging). The efficient chromatographic separation was achieved using a ZORBAX Eclipse XDB-C18 column (4.6×250 mm, 5 mm) with isocratic elution of mobile phase which consisted of acetonitrile:methanol:triethylamine solution (15:35:50, v/v/v) (pH 3.0). The flow rate of the mobile phase was 1 mL min-1, while the detection of amlodipine besylate was carried out at 273 nm. Amlodipine besylate and its impurity D were identified at the retention times of 16.529 min and 2.575 min, respectively. The linearity of the method with the coefficient of determination of 0.999 was confirmed in the concentration range of 10 - 75 µg mL-1 for amlodipine besylate. The limit of detection was 0.2 µg mL-1, while the limit of quantification was 0.66 µg mL-1. After UV and Vis radiation of the tablets packed in the primary packaging, the content of amlodipine besylate was reduced by 22.38% and 19.89%, respectively. The presence of new degradation products was not detected under the given chromatographic conditions. The photodegradation of amlodipine besylate followed pseudo-first-order kinetics. Based on the half-life of amlodipine besylate (38.4 days for UV radiation and 43.3 days for Vis radiation), it was concluded that amlodipine besylate in the tablets has satisfactory photostability after its packing in the Alu/PVC/PVDC blister packaging.

scholarly journals Rapid Determination of α-Hederin and Hederacoside C in Extracts of Hedera helix Leaves Available in the Czech Republic and Poland

2015 ◽  
Vol 10 (9) ◽  
pp. 1934578X1501000
Author(s):  
Lucie Havlíková ◽  
Kateřina Macáková ◽  
Lubomír Opletal ◽  
Petr Solich
Keyword(s):  
Mobile Phase ◽  
Ammonium Acetate ◽  
Rapid Determination ◽  
Hplc Method ◽  
Leaf Extracts ◽  
Hedera Helix ◽  
The Czech Republic ◽  
Upper Respiratory ◽  
Isocratic Mode

Leaf extracts of Hedera helix L. are widely used in the treatment of upper respiratory diseases. The saponins α-hederin and hederacoside C are considered to be the main compounds responsible for the biological activity. α-Hederin and hederacoside C were determined in H. helix leaf extracts using a fast, simple and validated HPLC method. An XTerra MS C18 column and mobile phase composed of 10 mM ammonium acetate at pH 8.5 (adjusted with triethylamine) and acetonitrile were used for the chromatography at 1.2 mL min−1. The column was kept at 30°C. Detection was performed at 220 nm. An approach utilizing a basic pH of the aqueous part of the mobile phase enabled analysis in 5 minutes in isocratic mode. The method was validated and used for the quality control of H. helix leaf ethanolic extracts.

scholarly journals Stability-Indicating Validated HPLC Method for Simultaneous Determination of Oral Antidiabetic Drugs from Thiazolidinedione and Sulfonylurea Groups in Combined Dosage Forms

2010 ◽  
Vol 93 (4) ◽  
pp. 1086-1092 ◽  
Author(s):  
Anna Gumieniczek ◽  
Anna Berecka ◽  
ukasz Komsta
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
Uv Light ◽  
Degradation Products ◽  
Dosage Forms ◽  
Hplc Method ◽  
Base Temperature ◽  
Stability Indicating ◽  
Acid And Base

Abstract For type 2 diabetes treatment, combinations of drugs from the thiazolidinedione and sulfonylurea groups are now available in the same tablet or capsule. Therefore, a stability-indicating and validated HPLC method was developed for simultaneous determination of pioglitazone, rosiglitazone, and glipizide in combined dosage forms. The examined drugs were subjected to different conditions such as acid and base, temperature, and UV light, and degradation of pioglitazone and glipizide was observed under thermal and acidic stress. However, selectivity of the presented method for pioglitazone, rosiglitazone, and glipizide assay against their degradation products was confirmed. It was also demonstrated to be robust, resisting small deliberate changes in pH of the buffer, flow rate, and percentage of acetonitrile in the mobile phase. The presented method utilizes a LiChrospher RP18 column (125 4.0 mm), acetonitrile in phosphate buffer at pH 4.3 (40 + 60, v/v) as the mobile phase, and UV detection at 225 nm for pioglitazone/glipizide or 245 nm for rosiglitazone/glipizide. The method was validated with respect to linearity, precision, and accuracy. Finally, the elaborated procedure was applied for the QC of pioglitazone/glipizide and rosiglitazone/glipizide mixtures.

scholarly journals Simultaneous HPLC Determination of Chlordiazepoxide and Mebeverine HCl in the Presence of Their Degradation Products and Impurities

2015 ◽  
Vol 2015 ◽  
pp. 1-9
Author(s):  
Rania N. El-Shaheny ◽  
Fathalla F. Belal
Keyword(s):  
Simultaneous Determination ◽  
Degradation Product ◽  
Mobile Phase ◽  
Degradation Products ◽  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Ir Studies ◽  
Validation Procedure

A simple, rapid, and sensitive RP-HPLC method was developed and validated for the simultaneous determination of chlordiazepoxide (CDO) and mebeverine HCl (MBV) in the presence of CDO impurity (2-amino-5-chlorobenzophenone, ACB) and MBV degradation product (veratric acid, VER). Separation was achieved within 9 min on a BDS Hypersil phenyl column (4.5 mm × 250 mm, 5 µm particle size) using a mobile phase consisting of acetonitrile: 0.1 M potassium dihydrogen phosphate: triethylamine (35 : 65 : 0.2, v/v/v) in an isocratic mode at a flow rate of 1 mL/min. The pH of the mobile phase was adjusted to 4.5 with orthophosphoric acid and UV detection was set at 260 nm. A complete validation procedure was conducted. The proposed method exhibited excellent linearity over the concentration ranges of 1.0–100.0, 10.0–200.0, 2.0–40.0, and 2.0–40.0 µg/mL for CDO, MBV, VER, and ACB, respectively. The proposed method was applied for the simultaneous determination of CDO and MBV in their coformulated tablets with mean percentage recoveries of 99.75 ± 0.62 and 98.61 ± 0.38, respectively. The results of the proposed method were favorably compared with those of a comparison HPLC method using Studentt-test and the variance ratioF-test. The chemical structure of MBV degradation product was ascertained by mass spectrometry and IR studies.

scholarly journals HPLC method for simultaneous determination of impurities and degradation products in Cardiazol

Pharmacia ◽  
2020 ◽  
Vol 67 (1) ◽  
pp. 29-37
Author(s):  
Iryna Drapak ◽  
Borys Zimenkovsky ◽  
Liudas Ivanauskas ◽  
Ivan Bezruk ◽  
Lina Perekhoda ◽  
...  
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Degradation Products ◽  
Phase 1 ◽  
Simultaneous Detection ◽  
Hplc Method ◽  
Column Temperature ◽  
Degree Of Separation ◽  
Determination Of Impurities

Aim. The aim of study was to develop a simple and accurate procedure that could be applied for the determination of impurities and degradation products in cardiazol. Materials and methods. Separation in samples was carried out with Acquity H-class UPLC system (Waters, Milford, USA) equipped with Acquity UPLC BEH C18 column (2.1 × 50 mm, 1.7 μm) (Waters, Milford, USA). Xevo TQD triple quadrupole mass spectrometer detector (Waters Millford, USA) was used to obtain MS/MS data. Mobile phase A: 0.1% solution of trifluoroacetic acid R in water R; Mobile phase B: acetonitrile R. Samples were chromatographed in gradient mode (Table 1). Flow rate of the mobile phase: 1 ml / min. Column temperature: 30 °С. Detection: at 240 nm wavelength. Injection volume: 10 μl. Results. The retention time of the main substance is about 18.5 minutes. The order of the peak, the retention times and relative retention times: impurity B (12.04, 0.65); impurity А (18.5; 0.98); Cardiazol (18.87; 1.00). The LOD and LOQ values obtained were in the range of 30 ng/mL to 100 ng/mL and 80 ng/mL to 310 ng/mL respectively (with respect to sample concentration of 2 mg/ml). Linearity was established in the range of LOQ level to 0.2% having regression coefficients in the range of 0.9996 to 0.9999. The change in the temperature of the column affects the degree of separation of cardiazol and the impurity A, and thus, with a decrease of 5 ° C, the degree of separation is (1.06), while with increasing this index (3.43). When changing the flow rate of the mobile phase, the degree of separation changes in the following order, with a decrease to 0.9 ml / min separation (1.90), with an increase in speed to 1.1 ml / min (2.45). When the number of mobile phase B decreases by 5%, the degree of separation varies by (2.65), with an increase of 5% (1.82). In comparison with the chromatogram of the tested solution, the substance is not resistant to the action of peroxide, alkaline and acid decomposition. Conclusion. 1) HPLC method was developed and validated for the simultaneous detection and quantitation of impurities formed during the synthesis of cardiazol. 2) The method proved to be sensitive, selective, precise, linear, accurate and stability-indicating.

scholarly journals Validated RP-HPLC Method for the Determination of Ivabradine Hydrochloride in Pharmaceutical Formulation

2017 ◽  
Vol 9 (05) ◽  
Author(s):  
MD. Muzaffar -ur- Rehman1 ◽  
G. Nagamallika
Keyword(s):  
Mobile Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Pharmaceutical Formulation ◽  
Intermediate Precision ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Bulk Drug

A simple, rapid, precise, and accurate RP-HPLC method for the estimation of Ivabradine Hydrochloride an anti-anginal agent, both as a bulk drug and in pharmaceutical formulation was developed. The chromatographic separation was achieved on a Thermosil C18 150 × 4.5 mm, 5μm column by using a mobile phase containing a mixture of methanol and phosphate buffer pH 6.5 in the ratio of 65:35 % v/v at a flow rate of 1ml/min and at an ambient temperature. The detection was monitored at a wavelength of 265nm. A clear chromatographic peak was identified with the retention time of 4.36 min and tailing factor of 1.23. The developed method was validated according to ICH guidelines with respect to specificity, linearity, accuracy, precision and robustness. The method shows a good linear relationship with correlation co-efficient of more than 0.992 in the concentration range of 30μg-150μg. The method showed mean % Recovery of 100.4% and %RSD for repeatability and intermediate precision was less than 2%. The proposed method can be used successfully for the quantitative determination of Ivabradine HCL in pharmaceutical dosage forms.

scholarly journals NOVEL HIGH-PERFORMANCE THIN-LAYER CHROMATOGRAPHIC METHOD FOR SIMPLE, ECONOMICAL, AND RAPID DETERMINATION OF FENOFIBRATE IN BULK AND PHARMACEUTICAL DOSAGE FORM

2018 ◽  
Vol 11 (5) ◽  
pp. 147
Author(s):  
Rani S Potawale ◽  
Tabassume I Hangad
Keyword(s):  
Thin Layer ◽  
Mobile Phase ◽  
High Performance ◽  
Regression Coefficient ◽  
Rapid Determination ◽  
High Sensitivity ◽  
Pharmaceutical Dosage Form ◽  
Densitometric Detection ◽  
Hptlc Method

 Objective: A simple, novel, sensitive, and rapid high-performance thin-layer chromatographic (HPTLC) method has been developed and validated for quantitative determination of fenofibrate in bulk and formulations.Methods: The chromatographic development was carried out on HPTLC plates precoated with silica gel 60 F254 using a single solvent dichloromethane as a simple mobile phase. Densitometric detection was carried out at 292 nm.Results: Rf value of drug was found to be 0.33±0.02. The method was validated as per International Conference on Harmonization Guideline with respect to linearity, accuracy, precision, and robustness. The calibration curve was found to be linear over a range of 20–400° ng band−1° with a regression coefficient of 0.999. The method has proved high sensitivity and specificity.Conclusion: Proposed densitometric method was found to be new, simple, and economic for routine quantification of fenofibrate in bulk and pharmaceutical formulation.

Stability-Indicating Spectrofluorometric Method for the Determination of Some Cephalosporin Drugs via Their Degradation Products

2015 ◽  
Vol 98 (2) ◽  
pp. 361-370 ◽  
Author(s):  
Nadia M Mostafa ◽  
Laila Abdel-Fattah ◽  
Soheir A Weshahy ◽  
Nagiba Y Hassan ◽  
Shereen A Boltia
Keyword(s):  
Degradation Products ◽  
Hplc Method ◽  
Excitation Wavelength ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Acid Degradation ◽  
Accuracy And Precision ◽  
Spectrofluorometric Method ◽  
Good Agreement

Abstract A stability-indicating spectrofluorometric method was investigated for the determination of three cephalosporin drugs, namely, cefpodoxime proxetil (CPD), cefixime trihydrate (CFX), and cefepime hydrochloride (CPM), via their acid and alkali degradation products. The three drugs were determined via their acid degradation at 432, 422, and 435 nm using an excitation wavelength of 310, 330, and 307 nm for CPD, CFX, and CPM determination, respectively, and via their alkali degradation at 407, 411, and 405 nm using an excitation wavelength of 310, 305, and 297 nm for CPD, CFX, and CPM determination, respectively. Linearity was achieved in the ranges of 0.35–3.50,0.4–4.0, and 0.3–3.0 μg/mL for the acid degradation products of CPD, CFX, and CPM, respectively, and in ranges of 0.05–0.5, 0.1–1.0, and 0.08–0.80 μg/mL for the alkali degradation products of CPD, CFX, and CPM, respectively. The method was validated for various parameters according to International Conference on Harmonization guidelines. The method was successfullyapplied for the determination of these cephalosporindrugs in pharmaceutical dosage forms with good accuracy and precision. The results obtained by the proposed spectrofluorometric method were compared with good agreement to the official HPLC method.

scholarly journals A Validated High-Performance Thin-Layer Chromatographic Method for the Simultaneous Determination of Zofenopril Calcium and Hydrochlorothiazide in the Presence of the Hydrochlorothiazide Impurities: Chlorothiazide and Salamide

2018 ◽  
Vol 101 (4) ◽  
pp. 1031-1041 ◽  
Author(s):  
Mamdouh R Rezk ◽  
Ahmed S Fayed ◽  
Hoda M Marzouk ◽  
Samah S Abbas
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Degradation Products ◽  
Raw Materials ◽  
Drug Product ◽  
Hplc Method ◽  
Pharmaceutical Formulation ◽  
Significant Difference ◽  
Hptlc Method

Abstract The chromatographic analysis of either process-related impurities or degradation products is very important in the pharmaceutical industry. In this work, a simple, selective, and sensitive HPTLC method was developed and validated for the simultaneous determination of zofenopril calcium (ZOF) and hydrochlorothiazide (HCT) in the presence of the HCT impurities: A) chlorothiazide (CT) and B) salamide, in raw materials and in pharmaceutical formulation. The separation was carried out on HPTLC silica gel 60 F254 using ethyl acetate–glacial acetic acid–triethylamine (10 + 0.1 + 0.1, v/v/v) as a developing system. The separated bands were scanned densitometrically at 270 nm. Polynomial equations were used for the regression. Calibration curves were constructed for ZOF, HCT, CT, and salamide in the ranges of 0.5–10, 0.2–4, 0.05–1.4, and 0.05–1.0 μg/band, respectively. Different parameters affecting the suggested method, including developing systems of varying composition/ratios and different detection wavelengths, were studied to achieve the best resolution and precision with good sensitivity. System suitability parameters were also tested. The proposed method was validated as per the International Conference on Harmonization guidelines and was successfully applied for the quantification of the studied drugs in their pharmaceutical formulation, with no interference from excipients observed. The results obtained by the developed HPTLC method were compared statistically with those obtained by the reported HPLC method using Student’s t and F ratio tests, and no significant difference was obtained, indicating the ability of the proposed method to be used for routine analysis of drug product.

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