- Department of Pharmaceutical Chemistry Faculty of Pharmacy, University of Karachi, Karachi
- +92-021-34664402
A novel reversed-phase liquid chromatographic method with UV detection for rapid and accurate simultaneous quantitation of prazosin (PRZ) and the key calcium channel blockers (CCBS), amlodipine besylate (AML), diltiazem hydrochloride... more
A novel reversed-phase liquid chromatographic method with UV detection for rapid and accurate simultaneous
quantitation of prazosin (PRZ) and the key calcium channel blockers (CCBS), amlodipine besylate (AML), diltiazem
hydrochloride (DIL) and verapamil hydrochloride (VER) in active pharmaceutical ingredients, pharmaceutical dosage
formulations and human serum has been developed and validated according to ICH guidelines.
The reduced run time and low cost of analysis are additional merits of the method. This method showed the best
resolution by using pre-packed Nucleosil® C18 (10 μm, 25 × 0.46 cm) column at ambient temperature. The mobile
phase consisting of methanol:water:acetonitrile (55:35:10 v/v; pH adjusted to 2.65 with phosphoric acid) was pumped
at a flow rate of 1.0 mL min-1 with an average operating pressure of 130 kg/cm2 and effluent was monitored at 238 nm.
Linearity of the method in the concentration range 5-100 μg mL-1 for prazosin and 10-600 μg mL-1 for calcium channel
blockers showed good linear relationships for all the analytes (R2
< 0.9998). The LLOD values were 32.8, 30.6, 54.2,
29.9 and LLOQ were 99.4, 92.6, 164.2, 90.5 ng mL-1 for PRZ, AML, DIL and VER respectively, as per ICH guide lines
acceptance criteria of 98 - 102%.
The newly developed method has been successfully employed for studying the interactions between prazosin and
ca-channel blockers at simulated human body conditions; the results envisage a positive interaction between the two
classes of drugs, as the percent recovery of the drugs almost changed, which indicate that prazosin may not be safe
to co-administer with these antihypertensive drugs
quantitation of prazosin (PRZ) and the key calcium channel blockers (CCBS), amlodipine besylate (AML), diltiazem
hydrochloride (DIL) and verapamil hydrochloride (VER) in active pharmaceutical ingredients, pharmaceutical dosage
formulations and human serum has been developed and validated according to ICH guidelines.
The reduced run time and low cost of analysis are additional merits of the method. This method showed the best
resolution by using pre-packed Nucleosil® C18 (10 μm, 25 × 0.46 cm) column at ambient temperature. The mobile
phase consisting of methanol:water:acetonitrile (55:35:10 v/v; pH adjusted to 2.65 with phosphoric acid) was pumped
at a flow rate of 1.0 mL min-1 with an average operating pressure of 130 kg/cm2 and effluent was monitored at 238 nm.
Linearity of the method in the concentration range 5-100 μg mL-1 for prazosin and 10-600 μg mL-1 for calcium channel
blockers showed good linear relationships for all the analytes (R2
< 0.9998). The LLOD values were 32.8, 30.6, 54.2,
29.9 and LLOQ were 99.4, 92.6, 164.2, 90.5 ng mL-1 for PRZ, AML, DIL and VER respectively, as per ICH guide lines
acceptance criteria of 98 - 102%.
The newly developed method has been successfully employed for studying the interactions between prazosin and
ca-channel blockers at simulated human body conditions; the results envisage a positive interaction between the two
classes of drugs, as the percent recovery of the drugs almost changed, which indicate that prazosin may not be safe
to co-administer with these antihypertensive drugs
Research Interests:
Mirza AZ, Arayne MS, Sultana N and Quraishi F (2013) Spectroscopic Study to Characterize In vitro Interaction of Losartan with Gliquidone and Pioglitazone Medicinal Chemistry Research 22 (1) 351-359 (2013) DOI: 10.1007/s00044-012-0036-8 http://link.springer.com/article/10.1007%2Fs00044-012-0036-8more
Research Interests:
Arthritic rats
Research Interests:
Research Interests:
A simple reversed phase HPLC method has been successfully developed and validated for the quantitative determination of levofloxacin (LVX) in bulk material, pharmaceutical formulation and serum. Purospher STAR C18 (25 cm x 4.6 mm, 5 μ m)... more
A simple reversed phase HPLC method has been successfully developed and validated for the quantitative determination of levofloxacin (LVX) in bulk material, pharmaceutical formulation and serum. Purospher STAR C18 (25 cm x 4.6 mm, 5 μ m) was used. The mobile phase MeOH: H2O (70:30, v/v) was delivered at a flow rate of 1 Ml min-1. The proposed method is specific, accurate with a recovery of 100 0.02. The detection limits were 2 ng with an RSD 0.1 (n=6).The anticipated method is applicable to routine analysis of LVX in pharmaceutical formulations and human serum samples. The method was applied to study the In vitro availability of levofloxacin in presence of various elements essential to the human body, like magnesium, calcium, chromium, copper Zinc and iron. The availability of Levofloxacin in presence of these elements was depressed up to 21% in simulated gastric juice, while up to 5% in pH 7.4 and 27% in simulated intestinal juice.
Research Interests:
Pregabalin an antiepileptic was the first compound approved by FDA for treating chronic pain. A sensitive, efficient, economical, environmental friendly and isocratic liquid chromatographic method for the determination of pregabalin in... more
Pregabalin an antiepileptic was the first compound approved by FDA for treating chronic pain. A sensitive,
efficient, economical, environmental friendly and isocratic liquid chromatographic method for the determination
of pregabalin in bulk drug, pharmaceutical dosage forms and human serum has been developed and validated
according to ICH guidelines.
Chromatographic separation was performed on a KROMASIL® 100-5 C-18 column (250×4.6 i.d. mm) (5 μm
particle size) as stationary phase with a UV detection at 210 nm using isocratic elution when buffer pH 7 and
acetonitrile (96:4, v/v) were used as the mobile phase and the flow rate was 1 ml min-1 at ambient temperature,the
retention time was 4.6 minutes.The method showed good linearity in the range 1-25 μg mL-1 with R2>0.999. The
lower limit of detection (LLOD) and quantitation (LLOQ) were 10 ng mL-1 and 17 ng mL-1 and 0.04 and 0.12 ng mL-1
for drug and serum, respectively.
Validation of the method showed good precision and accuracy for the proposed method. The newly developed
method can be successfully applied for the determination of pregabalin in active pharmaceutical ingredients,
pharmaceutical formulations, human serum and could be used in therapeutic drug monitoring and clinical laboratories
without diode array detector and without interference of excipients or endogenous components of serum.
efficient, economical, environmental friendly and isocratic liquid chromatographic method for the determination
of pregabalin in bulk drug, pharmaceutical dosage forms and human serum has been developed and validated
according to ICH guidelines.
Chromatographic separation was performed on a KROMASIL® 100-5 C-18 column (250×4.6 i.d. mm) (5 μm
particle size) as stationary phase with a UV detection at 210 nm using isocratic elution when buffer pH 7 and
acetonitrile (96:4, v/v) were used as the mobile phase and the flow rate was 1 ml min-1 at ambient temperature,the
retention time was 4.6 minutes.The method showed good linearity in the range 1-25 μg mL-1 with R2>0.999. The
lower limit of detection (LLOD) and quantitation (LLOQ) were 10 ng mL-1 and 17 ng mL-1 and 0.04 and 0.12 ng mL-1
for drug and serum, respectively.
Validation of the method showed good precision and accuracy for the proposed method. The newly developed
method can be successfully applied for the determination of pregabalin in active pharmaceutical ingredients,
pharmaceutical formulations, human serum and could be used in therapeutic drug monitoring and clinical laboratories
without diode array detector and without interference of excipients or endogenous components of serum.
Abstract Background: Rheumatoid arthritis is an autoimmune disorder in which patients not only suffer from joint misery but also face its associated depression. Objectives: To evaluate the anti-arthritic effects of leflunomide (5... more
Abstract
Background: Rheumatoid arthritis is an autoimmune disorder in which patients not only suffer from joint misery but
also face its associated depression.
Objectives: To evaluate the anti-arthritic effects of leflunomide (5 mg.kg-1.day-1) and meloxicam (5 mg.kg-1.day-1)
when given together on progression of rheumatoid arthritis and its associated depression in Adjuvant-Induced Arthritic
(AIA) rats.
Methodology: AIA was induced in female Sprague-Dawley rats. Paw volumes was measured to evaluate arthritic
progression while brain indolamines (tryptophan, serotonin and its metabolite 5-hydroxyindoleacetic acid) were
estimated by HPLC-EC method to determine associated depression. Leflunomide and meloxicam were given orally and
intraperitoneally throughout the experiment.
Results: Leflunomide and meloxicam inhibited RA progression significantly (p<0.005), in terms of joint erythema
and limb swelling, when given alone but fail to do so in combination in contrast to untreated or saline-treated arthritic
rats. Significant reduction (p<0.005) in all brain indolamines levels was found in all arthritic rats when compared with
normal. Furthermore, treatment with leflunomide and meloxicam alone or mutually significantly decrease (p<0.005)
brain indolamines level in comparison with untreated or saline-treated arthritic rats.
Conclusion: Leflunomide and meloxicam though reduces RA progression when given alone but in combined
therapy produce severe adverse effect. Depression is prominent with RA and therapy with leflunomide and meloxicam
exaggerate the conditions.
Background: Rheumatoid arthritis is an autoimmune disorder in which patients not only suffer from joint misery but
also face its associated depression.
Objectives: To evaluate the anti-arthritic effects of leflunomide (5 mg.kg-1.day-1) and meloxicam (5 mg.kg-1.day-1)
when given together on progression of rheumatoid arthritis and its associated depression in Adjuvant-Induced Arthritic
(AIA) rats.
Methodology: AIA was induced in female Sprague-Dawley rats. Paw volumes was measured to evaluate arthritic
progression while brain indolamines (tryptophan, serotonin and its metabolite 5-hydroxyindoleacetic acid) were
estimated by HPLC-EC method to determine associated depression. Leflunomide and meloxicam were given orally and
intraperitoneally throughout the experiment.
Results: Leflunomide and meloxicam inhibited RA progression significantly (p<0.005), in terms of joint erythema
and limb swelling, when given alone but fail to do so in combination in contrast to untreated or saline-treated arthritic
rats. Significant reduction (p<0.005) in all brain indolamines levels was found in all arthritic rats when compared with
normal. Furthermore, treatment with leflunomide and meloxicam alone or mutually significantly decrease (p<0.005)
brain indolamines level in comparison with untreated or saline-treated arthritic rats.
Conclusion: Leflunomide and meloxicam though reduces RA progression when given alone but in combined
therapy produce severe adverse effect. Depression is prominent with RA and therapy with leflunomide and meloxicam
exaggerate the conditions.
Research Interests:
A highly sensitive LC method with UV detection has been developed for the simultaneous determination of coadministered drugs captopril, piroxicam, and amlodipine in bulk drug, pharmaceutical formulations, and human serum at the isosbestic... more
A highly sensitive LC method with UV detection has been developed for the simultaneous determination of coadministered drugs captopril, piroxicam, and amlodipine in bulk drug, pharmaceutical formulations, and human serum at the isosbestic point (235 nm) and at individual λmax (220, 255, and 238 nm, respectively) by programming the detector with time to match the individual analyte's chromophore, which enhanced the sensitivity with linear range. The assay involved an isocratic elution of analytes on a Bondapak C18 (10 μm, 25 × 0.46 cm) column at ambient temperature using a mobile phase of methanol/water 80:20 at pH 2.9 and a flow rate of 1.0 mL/min. Linearity was found to be 0.25–25, 0.10–6.0, and 0.20–13.0 μg/mL with correlation coefficient >0.998 and detection limits of 7.39, 3.90, and 9.38 ng/mL, respectively, whereas calibration curves for wavelength-programmed analysis were 0.10–6.0, 0.04–2.56, and 0.10–10.0 μg/mL with correlation coefficient >0.998 and detection limits of 5.79, 2.68, and 3.87 ng/mL, respectively. All the validated parameters were in the acceptable range. The recovery of drugs was 99.32–100.39 and 98.65–101.96% in pharmaceutical formulation and human serum, respectively, at the isosbestic point and at individual λmax. This method is applicable for the analysis of drugs in bulk drug, tablets, serum, and in clinical samples without interference of excipients or endogenous serum components.
Sultana N, Arayne MS, (2013) 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 American Journal of Analytical Chemistry (AJAC) 4(1) 24-33. more