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Chinese Journal of Chemistry 2011年第6期29卷 1216-1220页

作者： najma, sultana Arayne, M. Saeed Safila, Naveed United Biotechnologies Karachi-75290 Pakistan Faculty of Pharmacy Hamdard University Karachi-74600 Pakistan

Lisinopril is found to be useful in hypertension and statins as cholesterol lowering drug. Present work was designed for the simultaneous determination of lisinopril in presence of pravastatin, atorvastatin, and rosuvastatin using RP-HPLC method. A Purospher star C 18 （5 μm, 25 × 0.46 cm） column was used with mobile phase consisting of acetonitrile ： water （60 ： 40 V/V, pH 3.0） with flow rate of 1.0 mLomin-1 and the quantitative evaluation was performed at 225 nm. The retention time of lisinopril was 2.0 min and for pravastatin, rosuvastatin and atorvastatin was found to be 3.1, 4.5 and 8.3 min respectively. Suitability of this method for the quantitative determination of the drugs was proved by validation in accordance with the requirements laid down by International Conference on Harmonization （ICH） guidelines. Application of the suggested procedures were successfully applied to the determination of these compounds in active pharmaceutical ingredient and in pharmaceutical preparations, with high percentage of recovery, good accuracy and precision.

关键词： Lisinopril statins method validation HPLC determination

Development and Validation of a Liquid Chromatographic Method for the Determination of Leflunomide： Application to in vitro Drug Metal Interactions

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Chinese Journal of Chemistry 2011年第9期29卷 1933-1938页

作者： sultana, najma Muhammad, Saeed Arayne Khan, Moona Mehboob Nawaz, Muhammd United Biotechnologies Karachi 75290 Pakistan Jinnah Medical and Dental College Karachi Pakistan Department of Chemistry College of Science UAE University A1-Ain P.O. Box 17551 UAE

Leflunomide is a leading drug for the treatment of rheumatoid arthritis. The principle aim of this study was to develop and validate an RP-HPLC method for the determination of leflunomide in bulk and pharmaceutical dosage form using diclofenac sodium as an internal standard. For this purpose, chromatography was accomplished on a Purospher Start, C18 （5 μm, 12.5 cm×0.46 cm） column at ambient temperature. Methanol ： water （80 ： 20, V/V） solvent system was selected as mobile phase, the pH of which was adjusted to 3.4 by ortho-phosphoric acid and de- livered at a flow rate of 1.2 mLomin-1. Seperation of leflunomide and diclofenac sodium was carried out on a Purospher Start, C18 equipped with a UV-visible detector at 248 nm. The suitability of the method for the quantita- tive determination of the drugs is proven by validation in accordance with the requirements laid down by the Inter- national Conference on Harmonization （ICH） guidelines. The method was accurate （99.55%--100.03%）, specific, linear （R2〉0.999） and precise （intra-day precision 0.023%--0.93% and inter-day precision 0.26%--0.944%） in the range of 0.5--20 μg·mL^-1. The minimum limit of detection and quantification in pharmaceutical formulation were 0.05 and 0.15 μ***^-1, respectively. Thus the proposed method is simple, accurate, reproducible and suitable for the routine analysis of leflunomide in pharmaceutical formulations and was applied to study in vitro drug-metal interactions.

关键词： leflunomide liquid chromatography analytical method in vitro interaction metal

Synthesis and antibacterial studies of ciprofloxacin-metal complexes

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Journal of Chinese Pharmaceutical Sciences 2019年第6期28卷 422-429页

作者： najma sultana M.Saeed Arayne Ahsan Zamir Siddiqi Agha Zeeshan Mirza Research Institute of Pharmaceutical Sciences Department of Pharmaceutical ChemistryFaculty of PharmacyUniversity ofKarachiKarachi-75270Pakistan Department of Chemistry University of Karachi Chemistry Department Faculty of Applied SciencesUmm Al-Qura UniversityMakkahSaudi Arabia Research Laboratories Centre Faculty of Applied SciencesUmm Al-Qura UniversityMakkahSaudi Arabia

Metal complexes of ciprofloxacin were synthesized to study the effect of the drug on the metals present in the body or metals co-administered as multivitamin therapy. These complexes were then characterized by IR, UV, 1 H NMR, CHN and AA analyses. It was found that the metals coordinated through the β-keto carboxylic group, forming four coordinated complexes having square planar geometry. The effect of the antibacterial activity of these complexes with respect to parent drug was also studied against 14 different Gram + ve and Gram – ve organisms by the disk susceptibility technique. Some complexes showed improve activity as compared with the stated drug.

关键词： Ciprofloxacin IR UV ~1H NMR CHN AA analysis

高效液相色谱-紫外检测法同时测定药物制剂及人体血清中的奥美沙坦酯和厄贝沙坦及氢氯噻嗪(英文)

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色谱 2008年第5期26卷 544-549页

作者： sultana najma ARAYNE M Saeed ALI S Shahid SAJID Shahnawaz Department of Pharmaceutical Chemistry Research Institute of Pharmaceutical SciencesFaculty of PharmacyUniversity of Karachi Department of Chemistry Faculty of ScienceUniversity of Karachi

A simple,selective,sensitive,precise,simultaneous high performance liquid chromatographic analysis of serum samples and commercial tablet formulation containing hydrochlorothiazide,olmesartan medoxomil and irbesartan are *** chromatographic separation was achieved using a μ-Bondapak,C18 column(15 cm×4.6 mm,5 μm),and a mobile phase consisting of acetonitrile-0.2% acetic acid aqueous solution(50∶50,v/v)at a flow rate of 1.0 mL/*** ultraviolet detector was set at a wavelength of 260 ***,olmesartan medoxomil,and irbesartan were eluted at 1.2,3.8,and 4.4 min,*** extraneous materials were found to *** method uses protein precipitation with acetonitrile for the preparation of serum *** linear ranges for hydrochlorothiazide,olmesartan medoxomil,and irbesartan were 6.25-18.75,20-60,and 75-225 ng/mL,*** recoveries of hydrochlorothiazide,olmesartan medoxomil,and irbesartan in spiked samples were all greater than 98%,and their relative standard deviations were less than 2.0%.The limits of detection were 1,2,and 2 ng/mL for hydrochlorothiazide,olmesartan medoxomil,and irbesartan,respectively,and the limits of quantification were 3 ng/mL,which allow their determination at the expected serum concentration levels.

关键词：二氢氯噻色谱血清药物化学分析分析方法

An Ultra-sensitive LC Method for the Simultaneous Determination of Paracetamol, Carbamazepine, Losartan and Ciprofloxacin in Bulk Drug, Pharmaceutical Formulation and Human Serum by Programming the Detector

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American Journal of Analytical Chemistry 2013年第1期4卷 24-33页

作者： najma sultana Muhammad Saeed Arayne Saeeda Nadir Ali Department of Chemistry University of Karachi Karachi Pakistan Department of Pharmaceutical Chemistry Faculty of Pharmacy University of Karachi Karachi Pakistan

An ultra-sensitive LC method for the simultaneous quantitation of paracetamol, carbamazepine, losartan and ciprofloxacin have been developed and validated following the ICH guidelines at isobestic point and by programming the detector at individual wavelength of each component. The components were eluted by 50:50 v/v acetonitrile-water (pH 3.0) using a Bondapak, C18 (10 μm, 25 × 0.46 cm) column at flow rate of 1.0 mL·min-1 with detection wavelength 240 nm at isobestic point and 245, 230, 206 and 272 nm for paracetamol, carbamazepine, losartan potassium and ciprofloxacin respectively by programming the detector. Linearity was found to be 0.5 - 24, 0.25 - 8.0, 0.4 - 12 and 0.75 - 10 μg·mL-1 (R2 > 0.999) with detection limits 99, 20, 30 and 6.0 ng·mL-1 respectively. Comparison study with time program method showed more sensitivity with calibration range of 0.4 - 12, 0.2 - 6.0, 0.1 - 3.0 and 0.25 - 8.0 μg·mL-1 (R2 > 0.999) and LOD values 29, 11, 2.0 and 5.0 ng·mL-1 respectively. Percent recoveries >98.37% from pharmaceutical formulation and human serum samples and RSD 2% for inter-day and intra-day assay were obtained. The method was found to be robust and can be successfully applied for the determination of studied drugs in, pharmaceutical formulations and human serum without interference of excipients or endogenous components of serum.

关键词： Paracetamol Carbamazepine Losartan Ciprofloxacin Time Program

In vivo and in vitro interaction studies of ibuprofen with enalapril

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Journal of Coastal Life Medicine 2016年第4期4卷 327-330页

作者： Safila Naveed najma sultana Muhammad Saeed Arayne Research Institute of Pharmaceutical Sciences Faculty of Pharmacy University of KarachiKarachi-75270Pakistan Faculty of Pharmacy Jinnah University for WomenKarachiPakistan Department of Chemistry University of KarachiKarachiPakistan

Objective:To study the in vitro interactions of ibuprofen with ***:In this study,we investigated synergistic effect of angiotensin-converting enzyme inhibitor(enalapril)with commonly used nonsteroidal anti-inflammatory drug,ibuprofen in carrageenan induced inflammation ***-inflammatory response was observed for ibuprofen when given simultaneously with enalapril by comparing decrease in paw ***:The results were expressed in percentage reduction in paw size for every hour and were calculated for edema rate and percentage reduction in *** vitro interaction studies were carried out using high performance liquid chromatography and both the drugs were analyzed by assaying both drugs alone and in *** combination of enalapril and ibuprofen showed increased action of ibuprofen as shown by the increase of percentage reduction and decrease in edema *** was also proved from analytical ultracentrifugation of the chromatogram of combining ***:This learning has certain restriction as a number of experienced animals were small and the period of inflammatory response was checked for ibuprofen alone and simultaneous with enalapril for 5 *** studies may be required to establish the strong relationship.

关键词： Interaction Ibuprofen Enalapril High performance liquid chromatography

Simultaneous Determination of Amlodipine with H<sub>1</sub>-Receptor Antagonists by Reversed Phase High Performance Liquid Chromatography and Application to Interaction Studies

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American Journal of Analytical Chemistry 2012年第9期3卷 632-637页

作者： Muhammad Saeed Arayne najma sultana Saima Sher Bahadur Muhammad Nawaz Department of Chemistry United Arab Emirates University Al-Ain UAE Department of Chemistry University of Karachi Karachi Pakistan Research Institute of Pharmaceutical Sciences Department of Pharmaceutical Chemistry Faculty of Pharmacy University of Karachi Karachi Pakistan

A rapid, fast and precise method has been developed and validated for the simultaneous determination of amlodipine with H1-receptor antagonists (cetirizine, fexofenadine, and buclizine) from dosage forms. The chromatography was performed on a Purospher? Star, C18 (5 mm, 250 × 4.6 mm) column using acetonitrile: buffer (0.01 mM) (40:60, v/v, pH adjusted to 3.0), as a mobile phase. The mobile phase was pumped at a flow rate of 1.0 mL·min-1 and UV detection was performed at 240 nm. The method was validated for linearity, accuracy, precision and specificity. The method was applied to study the interaction between amlodipine and H1-receptor antagonists. These interactions were carried out in simulated gastric juice (pH 1), simulated full stomach (pH 4), blood pH (pH 7.4) and simulating GI (pH 9). The interacting drugs were heated at 37℃ with intermit-tent shaking and the samples were withdrawn every thirty minutes for three hours and drug contents were analyzed by RP-HPLC techniques. In most cases the in vitro availability of amlodipine was decreased. It was observed that the change in in vitro availability was pH dependent.

关键词： Amlodipine Cetirizine Fexofenadine Buclizine Interactions Reversed Phase High Performance Liquid Chromatography

RP-HPLC Method for the Simultaneous Determination of Lisinopril and NSAIDs in API, Pharmaceutical Formulations and Human Serum

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American Journal of Analytical Chemistry 2012年第2期3卷 147-152页

作者： najma sultana M. Saeed Arayne Rubina Siddiqui Safila Naveed Fatima Jinnah Medical and Dental College Karachi Pakistan Jinnah University for Women Karachi Pakistan United Biotechnologies Karachi Pakistan

High performance liquid chromatographic method was developed valdated and applied for the simultaneous determi- nation of lisinopril and NSAIDs in bulk, pharmaceuticals formulations and human serum. A Purospher star C18 (5 μm, 25 × 0.46 cm) column was used with mobile phase consisting of methanol: water: acetonitrile (80:17.5:2.5 v/v, pH 3.0) and quantitative evaluation was performed at 225 nm with a flow rate of 1.0 mL?min–1. The retention time of lisinopril was 2.2 min while naproxen, flurbiprofen, diclofenac sodium and mefenamic acid were found to be 4.0, 4.5, 5.0 and 6.7 min respectively. Suitability of this method for the quantitative determination of the drugs was proved by validation in accordance with the requirements laid down by International Conference on Harmonization (ICH) guidelines. The method is selective, precise, accurate and can be used for analysis of pharmaceutical preparations in quality control and clinical laboratories.

关键词： Lisinopril NSAIDs Method Validation HPLC Determination

New Method for Optimization and Simultaneous Determination of Sparfloxacin and Non Steroidal Anti-Inflammatory Drugs: Its <i>In-Vitro</i>Application

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American Journal of Analytical Chemistry 2012年第4期3卷 328-337页

作者： Somia Gul najma sultana Muhammad Saeed Arayne Sana Shamim Mahwish Akhtar College of Pharmacy Dow University of Health Sciences Karachi Pakistan Faculty of Pharmacy Jinnah University for Women Karachi Pakistan United Biotech (Pvt) Ltd. Karachi Pakistan

A simple reversed phase HPLC method was developed and validated for the simultaneous determination of sparfloxacin (SPFX), diclofenac sodium, meloxicam, ibuprofen, flurbiprofen, naproxen and mefenemic acid in a relatively short time with high linearity in bulk material, pharmaceutical formulations and human serum. Purospher STAR C18 (250 × 4.6 mm, 5 μm) column was utilized with mobile phase, methanol and water (90:10, v/v pH 2.70 adjusted by phosphoric acid), was delivered at a flow rate of 1.5 ***–1. Eluent was monitored using UV detector at 240 nm. The proposed method is specific, accurate (98.42% - 102.75%), precise (intra-day and inter-day variation 0.011% - 1.85%) and linear (R2 > 0.999) with in the desired range 0.15 - 40 μ***–1 and the detection and quantification limit was 1.19E+08 – 0.150 μ***–1 and 3.62E+08 – 0.4574 μ***–1 respectively for SPFX and NSAIDs. The analysis of variance (ANOVA) and student’s t-test were applied to verify the results. The anticipated method is applicable to routine analysis of SPFX and NSAIDs in pharmaceutical formulations as well as in human serum samples. It has also applied on interaction of SPFX with NSAIDs.

关键词： Sparfloxacin NSAIDs HPLC Interactions ANOVA

Drug-Drug Interaction Studies of Levocetirizine with Atenolol

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Journal of Pharmacy and Pharmacology 2017年第3期5卷 118-124页

作者： Shafaque Mehboob Muhammad Azhar Mughal Khalid Aftab MoonaMehboob Khan najma sultana Syed Arayne Institute of Pharmaceutical Sciences Jinnah Sindh Medical University Karachi 75510 Pakistan Department of Pharmacology & Therapeutics Jinnah Sindh Medical University Karaehi 75510 Pakistan Department of Pharmacology & Therapeutics Islam Medical & Dental College Sialkot 51311 Pakistan Department of Pharmaceutical Chemistry Dow University of Health Sciences Karachi 74200 Pakistan Department of Pharmaceutical Chemistry Faculty of Pharmacy University of Karachi Karachi 75270 Pakistan

The objective of the study was to evaluate the drug-drug interaction studies of levoceterizine with atenolol. Calibration curve studies of working standard solutions of levocetirizine and atenolol （0.01-0.1 mmol） were scanned. Maxima appeared at 231 nm for levocetirizine and 224 nm for atenolol. The calibration curve obeyed Beer Lambert＇s Law. Lone availabilities of both the drugs were studied in pH 1, pH 4, pH 7.4 and pH 9 at 37℃ on B.P. （British Pharmacopoeia） dissolution apparatus. To study the drug-drug interaction of levocetirizine （5 mg tablet） and atenolol （100 mg tablet）, both the drugs were introduced to the dissolution apparatus in simulated gastric juice （pH 1）, pH 4, pH 7.4 and pH 9 at 37℃ at zero time and measured the absorbance maxima of both the drugs at the corresponding wavelength. Graphs were plotted for availability percentage （%） of drug versus time at each set of experiment. The availability percentage （%） of levocetirizine in the buffers of pH simulated to gastric pH 4, pH 7.4 and pH 9 in the presence of atenolol was 436.78%, 376.90%, 436.78% and 436.78%, respectively, but the availability of atenolol was increased up to 214.80%, 212.96%, 214.93% and 231.51% in simulated to gastric pH and in the buffers ofpH 4, pH 7.4 and pH 9, respectively. On the basis of these studies, it is concluded that levocetirizine forms a charge-complex with atenolol; therefore, co-administration of these drugs should be avoided.

关键词： Levocetirizine atenolol drug-drug interactions absorbance maxima.