A sensitive and rapid liquid chromatography-tandem mass spectrometry(LC–MS/MS) method has been developed for the simultaneous determination of lisinopril(LIS) and hydrochlorothiazide(HCTZ) in human plasma using their...A sensitive and rapid liquid chromatography-tandem mass spectrometry(LC–MS/MS) method has been developed for the simultaneous determination of lisinopril(LIS) and hydrochlorothiazide(HCTZ) in human plasma using their labeled internal standards(ISs). Sample pre-treatment involved solid phase extraction on Waters Oasis HLB cartridges using 100 μL of plasma, followed by liquid chromatography on Hypersil Gold C_(18)(50 mm×3.0 mm, 5 μm) column. The analytes were eluted within 2.0 min using acetonitrile-5.0 m M ammonium formate, p H 4.5(85:15, v/v) as the mobile phase. The analytes and ISs were analyzed in the negative ionization mode and quantified using multiple reaction monitoring. The method showed excellent linearity over the concentration range of 0.50–250.0 ng/m L for both the analytes. The intra-batch and inter-batch precision(% CV) was ≤5.26% and their extraction recoveries were in the range of 96.6%–103.1%. Matrix effect evaluated in terms of IS-normalized matrix factors ranged from 0.97 to 1.03 for both the analytes. The validated method was successfully applied to determine the plasma concentration of the drugs using 10 mg lisinopril and 12.5 mg hydrochlorothiazide fixed dose formulation in 18 healthy Indian volunteers.展开更多
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 C...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.展开更多
During the routine impurity profile of lisinopril bulk drug by HPLC (high-performance liquid chromatography), a potential impurity was detected. Using multidimensional NMR (nuclear magnetic resonance) technique, the t...During the routine impurity profile of lisinopril bulk drug by HPLC (high-performance liquid chromatography), a potential impurity was detected. Using multidimensional NMR (nuclear magnetic resonance) technique, the trace-level impurity was unambiguously identified to be 2-(-2-oxo-azocan-3-ylamino)-4-phenyl-butyric acid after isolation from lisinopril bulk drug by semi-preparative HPLC. Formation of the impurity was also discussed. To our knowledge, this is a novel impurity and not reported elsewhere.展开更多
Two trace impurities in the bulk drug lisinopril were detected by means of high-performance liquid chromatography coupled with mass spectrometry （HPLC/MS） with a simple and sensitive method suitable for HPLC/MSn ana...Two trace impurities in the bulk drug lisinopril were detected by means of high-performance liquid chromatography coupled with mass spectrometry （HPLC/MS） with a simple and sensitive method suitable for HPLC/MSn analysis. The fragmentation behavior of lisinopfil and the impurities was investigated, and two unknown impurities were elucidated as 2-（6-amino- l-（l-carboxyethylamino）- l-oxohexan-2-ylamino）-4-phenylbutanoic acid and 6-amino-2-（l-carboxy-3-phenylpropylamino）-hexanoic acid on the basis of the multi-stage mass spectrometry and exact mass evidence, The proposed structures of the two unknown impurities were further confirmed by nuclear magnetic resonance （NMR） experiments after preparative isolation.展开更多
A simple, precise, accurate and sensitive reverse phase high performance liquid chromatographic method for simultaneous estimation of lisinopril dihydrate and its degradation products occuring under different ICH pres...A simple, precise, accurate and sensitive reverse phase high performance liquid chromatographic method for simultaneous estimation of lisinopril dihydrate and its degradation products occuring under different ICH prescribed stress conditions has been modified. Drug was resolved on a C18 column, utilizing modified mobile phase of tetra butyl ammonium hydroxide solution and acetonitrile. Ultra violet detection was carried out at 210 nm. The method was modified with respect to linearity, precision, accuracy, selectivity, specificity and ruggedness. The results obtained revealed that lisinopril dihydrate was an active product slightly changed under stress conditions.展开更多
<span style="font-family:Verdana;">A sensitive and eco-friendly method was developed for the spectrophotometric determination of Lisinopril (LSP) in bulk and pharmaceutical formulations by cloud point ...<span style="font-family:Verdana;">A sensitive and eco-friendly method was developed for the spectrophotometric determination of Lisinopril (LSP) in bulk and pharmaceutical formulations by cloud point extraction technique. The method was based on the formation of a blue</span><span style="font-family:Verdana;">-</span><span style="font-family:Verdana;">colored coordination complex between Lisinopril (LSP) and Cobalt Thiocyanate (CTC) at a suitable pH.</span><span style="font-family:""> </span><span style="font-family:""><span style="font-family:Verdana;">The Complex in aqueous medium</span><span style="font-family:Verdana;"> was extracted into surfactant layer by cloud point extraction using</span><span style="font-family:Verdana;"> a non-ionic surfactant Triton X-114 and then the surfactant layer was dissolved in a suitable volume of ethanol and the amount of Lisinopril was determined spectrophotometrically at a wavelength of 625</span></span><span style="font-family:""> </span><span style="font-family:Verdana;">nm.</span><span style="font-family:""> </span><span style="font-family:""><span style="font-family:Verdana;">The conditions like concentration of the drug, concentration of CTC and of Triton X-114, P</span><sup><span style="font-family:Verdana;">H</span></sup></span><span style="font-family:Verdana;">,</span><span style="font-family:Verdana;"> etc. were optimized by OFAT (One Factor At a Time) method. The linear range of calibration curve was 1</span><span style="font-family:""> </span><span style="font-family:Verdana;">-</span><span style="font-family:""> </span><span style="font-family:Verdana;">6 μg/ml and the linear regression equation with a correlation coefficient of 0.99996 was y = 0.0021</span><span style="font-family:""> </span><span style="font-family:Verdana;">+</span><span style="font-family:""> </span><span style="font-family:Verdana;">0.084x.</span><span style="font-family:""> </span><span style="font-family:Verdana;">Preconcentration and enrichment factors were found to be 100 and 3.12 respectively, achieving the detection limit of 0.0588</span><span style="font-family:""> </span><span style="font-family:Verdana;">μg/ml. The proposed method was successfully applied for the determination of LSP in the drug formulations. The obtained values were in agreement with the values as quoted by the manufacturers.展开更多
Angiotensin-converting enzyme inhibitor induced angioedema (AIIA) can vary from mild to life-threatening. A vast majority of cases of AIIA occur within a month of starting an angiotensin-converting enzyme-inhibitor (A...Angiotensin-converting enzyme inhibitor induced angioedema (AIIA) can vary from mild to life-threatening. A vast majority of cases of AIIA occur within a month of starting an angiotensin-converting enzyme-inhibitor (ACE-I). We present a 48-year-old male who presented with respiratory failure secondary to AIIA, after being on lisinopril for over 8 years. He had no previous complications secondary to lisinopril and aside from smoking, carried no risk factors for AIIA. Despite conventional treatment for angioedema, he had a prolonged stay in the Medical Intensive Care Unit (MICU). Following discharge, there hasn’t been a recurrence of AIIA since the discontinuation of lisinopril. The case is intended to caution that AIIA remains possible even late into a chronic regimen of ACE-I. This is a risk that shouldn’t be neglected, even with sparse risk factors or longer duration of ACE-I use. Conventional treatment is not currently in line with proposed etiologies of AIIA. We advocate for more clinical trials involving pharmaceutical agents targeting bradykinin accumulation.展开更多
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 rosuv...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.展开更多
In this study, we developed a simple and sensitive HPLC method for the determination of lisinopril in human plasma. The sample clean-up was carried out by solid-phase extraction(SPE) using a cation-exchange(Strata-SCX...In this study, we developed a simple and sensitive HPLC method for the determination of lisinopril in human plasma. The sample clean-up was carried out by solid-phase extraction(SPE) using a cation-exchange(Strata-SCX~?) extraction cartridge. After a pre-column derivatization with 4-fluoro-7-nitro-2,1,3-benzoxadiazole, the reaction mixture was analyzed on an Agilent Zorbax SB~?-C_(18)(150 mm×4.6 mm, 5 μm). The flow rate was set at 1.0 mL/min. Fluorescence detection was performed at an excitation wavelength of 470 nm and an emission wavelength of 530 nm. The mobile phase consisted of a mixture of methanol and 0.02 M sodium dihydrogen phosphate(pH = 3.0, 60:40, v/v). The average extraction recovery of lisinopril and fluvoxamine(internal standard) was >85%. The method exhibited a linear calibration curve over the concentration range of 1–1000 ng/mL with a correlation coefficient(r^2) of ≥0.98 and a limit of quantification(LOQ) equal to 2 ng/mL. The within-run and between-run precisions were satisfactory with an RSD of 3.8%–13.7%(accuracy: from 95.0% to 96.4%) and 4.273%–14.3%(accuracy: from 94.4% to 98.5%), respectively.展开更多
A rapid and practical method for direct detection of lisinopril in anion exchange chromatography（AEC） has been developed with integrated pulsed amperometric detection（IPAD）.Dionex AS 18（250 mm×2 mm） and AG...A rapid and practical method for direct detection of lisinopril in anion exchange chromatography（AEC） has been developed with integrated pulsed amperometric detection（IPAD）.Dionex AS 18（250 mm×2 mm） and AG 18（50 mm×2 mm） columns and 40 mmol/L NaOH solution were used for separation.Multi-step potential waveform parameters were optimized to maximize the signal-to-noise ratio（S/N）.Utilizing the optimized waveform,the repeatability（intra-day） precision and intermediate（inter-day） precision were obtained with relative standard deviation（RSD） of 0.74,0.93,respectively.The limit of quantification（LOQ） and limit of detection（LOD） were found to be 0.37,0.12ng/mL,respectively,with the correlation coefficient of 0.9998 over concentration range 0.01-1μg/mL.The present method was successfully applied to the determination of lisinopril in human plasma.The recoveries of plasma sample spiked by 0.2μg/mL,0.8μg/mL lisinopril were 98.31-103.23%with RSD of 1.41%, 0.61%,respectively.展开更多
基金University Grants Commission (UGC), New Delhi, India for BSR fellowship F 4-1/2009 (BSR)/7-74/2007the Department of Chemistry, Gujarat University
文摘A sensitive and rapid liquid chromatography-tandem mass spectrometry(LC–MS/MS) method has been developed for the simultaneous determination of lisinopril(LIS) and hydrochlorothiazide(HCTZ) in human plasma using their labeled internal standards(ISs). Sample pre-treatment involved solid phase extraction on Waters Oasis HLB cartridges using 100 μL of plasma, followed by liquid chromatography on Hypersil Gold C_(18)(50 mm×3.0 mm, 5 μm) column. The analytes were eluted within 2.0 min using acetonitrile-5.0 m M ammonium formate, p H 4.5(85:15, v/v) as the mobile phase. The analytes and ISs were analyzed in the negative ionization mode and quantified using multiple reaction monitoring. The method showed excellent linearity over the concentration range of 0.50–250.0 ng/m L for both the analytes. The intra-batch and inter-batch precision(% CV) was ≤5.26% and their extraction recoveries were in the range of 96.6%–103.1%. Matrix effect evaluated in terms of IS-normalized matrix factors ranged from 0.97 to 1.03 for both the analytes. The validated method was successfully applied to determine the plasma concentration of the drugs using 10 mg lisinopril and 12.5 mg hydrochlorothiazide fixed dose formulation in 18 healthy Indian volunteers.
文摘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.
基金Project (No. 20375036) supported partly by the National NaturalScience Foundation of China
文摘During the routine impurity profile of lisinopril bulk drug by HPLC (high-performance liquid chromatography), a potential impurity was detected. Using multidimensional NMR (nuclear magnetic resonance) technique, the trace-level impurity was unambiguously identified to be 2-(-2-oxo-azocan-3-ylamino)-4-phenyl-butyric acid after isolation from lisinopril bulk drug by semi-preparative HPLC. Formation of the impurity was also discussed. To our knowledge, this is a novel impurity and not reported elsewhere.
基金Project (No. 20772109) supported by the National Natural ScienceFoundation of China
文摘Two trace impurities in the bulk drug lisinopril were detected by means of high-performance liquid chromatography coupled with mass spectrometry （HPLC/MS） with a simple and sensitive method suitable for HPLC/MSn analysis. The fragmentation behavior of lisinopfil and the impurities was investigated, and two unknown impurities were elucidated as 2-（6-amino- l-（l-carboxyethylamino）- l-oxohexan-2-ylamino）-4-phenylbutanoic acid and 6-amino-2-（l-carboxy-3-phenylpropylamino）-hexanoic acid on the basis of the multi-stage mass spectrometry and exact mass evidence, The proposed structures of the two unknown impurities were further confirmed by nuclear magnetic resonance （NMR） experiments after preparative isolation.
文摘A simple, precise, accurate and sensitive reverse phase high performance liquid chromatographic method for simultaneous estimation of lisinopril dihydrate and its degradation products occuring under different ICH prescribed stress conditions has been modified. Drug was resolved on a C18 column, utilizing modified mobile phase of tetra butyl ammonium hydroxide solution and acetonitrile. Ultra violet detection was carried out at 210 nm. The method was modified with respect to linearity, precision, accuracy, selectivity, specificity and ruggedness. The results obtained revealed that lisinopril dihydrate was an active product slightly changed under stress conditions.
文摘<span style="font-family:Verdana;">A sensitive and eco-friendly method was developed for the spectrophotometric determination of Lisinopril (LSP) in bulk and pharmaceutical formulations by cloud point extraction technique. The method was based on the formation of a blue</span><span style="font-family:Verdana;">-</span><span style="font-family:Verdana;">colored coordination complex between Lisinopril (LSP) and Cobalt Thiocyanate (CTC) at a suitable pH.</span><span style="font-family:""> </span><span style="font-family:""><span style="font-family:Verdana;">The Complex in aqueous medium</span><span style="font-family:Verdana;"> was extracted into surfactant layer by cloud point extraction using</span><span style="font-family:Verdana;"> a non-ionic surfactant Triton X-114 and then the surfactant layer was dissolved in a suitable volume of ethanol and the amount of Lisinopril was determined spectrophotometrically at a wavelength of 625</span></span><span style="font-family:""> </span><span style="font-family:Verdana;">nm.</span><span style="font-family:""> </span><span style="font-family:""><span style="font-family:Verdana;">The conditions like concentration of the drug, concentration of CTC and of Triton X-114, P</span><sup><span style="font-family:Verdana;">H</span></sup></span><span style="font-family:Verdana;">,</span><span style="font-family:Verdana;"> etc. were optimized by OFAT (One Factor At a Time) method. The linear range of calibration curve was 1</span><span style="font-family:""> </span><span style="font-family:Verdana;">-</span><span style="font-family:""> </span><span style="font-family:Verdana;">6 μg/ml and the linear regression equation with a correlation coefficient of 0.99996 was y = 0.0021</span><span style="font-family:""> </span><span style="font-family:Verdana;">+</span><span style="font-family:""> </span><span style="font-family:Verdana;">0.084x.</span><span style="font-family:""> </span><span style="font-family:Verdana;">Preconcentration and enrichment factors were found to be 100 and 3.12 respectively, achieving the detection limit of 0.0588</span><span style="font-family:""> </span><span style="font-family:Verdana;">μg/ml. The proposed method was successfully applied for the determination of LSP in the drug formulations. The obtained values were in agreement with the values as quoted by the manufacturers.
文摘Angiotensin-converting enzyme inhibitor induced angioedema (AIIA) can vary from mild to life-threatening. A vast majority of cases of AIIA occur within a month of starting an angiotensin-converting enzyme-inhibitor (ACE-I). We present a 48-year-old male who presented with respiratory failure secondary to AIIA, after being on lisinopril for over 8 years. He had no previous complications secondary to lisinopril and aside from smoking, carried no risk factors for AIIA. Despite conventional treatment for angioedema, he had a prolonged stay in the Medical Intensive Care Unit (MICU). Following discharge, there hasn’t been a recurrence of AIIA since the discontinuation of lisinopril. The case is intended to caution that AIIA remains possible even late into a chronic regimen of ACE-I. This is a risk that shouldn’t be neglected, even with sparse risk factors or longer duration of ACE-I use. Conventional treatment is not currently in line with proposed etiologies of AIIA. We advocate for more clinical trials involving pharmaceutical agents targeting bradykinin accumulation.
文摘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.
基金The part of a Pham D thesis supported by Tehran University of Medical Sciences(Grant No.23049-92-02-92)
文摘In this study, we developed a simple and sensitive HPLC method for the determination of lisinopril in human plasma. The sample clean-up was carried out by solid-phase extraction(SPE) using a cation-exchange(Strata-SCX~?) extraction cartridge. After a pre-column derivatization with 4-fluoro-7-nitro-2,1,3-benzoxadiazole, the reaction mixture was analyzed on an Agilent Zorbax SB~?-C_(18)(150 mm×4.6 mm, 5 μm). The flow rate was set at 1.0 mL/min. Fluorescence detection was performed at an excitation wavelength of 470 nm and an emission wavelength of 530 nm. The mobile phase consisted of a mixture of methanol and 0.02 M sodium dihydrogen phosphate(pH = 3.0, 60:40, v/v). The average extraction recovery of lisinopril and fluvoxamine(internal standard) was >85%. The method exhibited a linear calibration curve over the concentration range of 1–1000 ng/mL with a correlation coefficient(r^2) of ≥0.98 and a limit of quantification(LOQ) equal to 2 ng/mL. The within-run and between-run precisions were satisfactory with an RSD of 3.8%–13.7%(accuracy: from 95.0% to 96.4%) and 4.273%–14.3%(accuracy: from 94.4% to 98.5%), respectively.
基金supported by the National Natural Science Foundation of China(Nos20775070,and 20911140271)the Natural Science Foundation of Zhejiang Province(NoR4080124)
文摘A rapid and practical method for direct detection of lisinopril in anion exchange chromatography（AEC） has been developed with integrated pulsed amperometric detection（IPAD）.Dionex AS 18（250 mm×2 mm） and AG 18（50 mm×2 mm） columns and 40 mmol/L NaOH solution were used for separation.Multi-step potential waveform parameters were optimized to maximize the signal-to-noise ratio（S/N）.Utilizing the optimized waveform,the repeatability（intra-day） precision and intermediate（inter-day） precision were obtained with relative standard deviation（RSD） of 0.74,0.93,respectively.The limit of quantification（LOQ） and limit of detection（LOD） were found to be 0.37,0.12ng/mL,respectively,with the correlation coefficient of 0.9998 over concentration range 0.01-1μg/mL.The present method was successfully applied to the determination of lisinopril in human plasma.The recoveries of plasma sample spiked by 0.2μg/mL,0.8μg/mL lisinopril were 98.31-103.23%with RSD of 1.41%, 0.61%,respectively.
