scholarly journals Determination of Atenolol and Trimetazidine in Pharmaceutical Tablets and Human Urine Using a High Performance Liquid Chromatography-Photo Diode Array Detection Method

2019 ◽  
Vol 2019 ◽  
pp. 1-8 ◽  
Author(s):  
Walaa El-Alfy ◽  
Omnia A. Ismaiel ◽  
Magda Y. El-Mammli ◽  
Abdalla Shalaby
Keyword(s):  
Human Urine ◽  
Limit Of Detection ◽  
Pure Form ◽  
Urine Samples ◽  
Dihydrogen Phosphate ◽  
Simple Liquid ◽  
Pharmaceutical Tablets ◽  
Limit Of Quantitation ◽  
Precision And Accuracy

A simple RP-HPLC-PDA method for determination of atenolol (ATN) and trimetazidine (TMZ) in human urine and tablets has been developed. Analytes were separated on a Caltrex BI column (125× 4.0 mm, 5 μm) with 25mM potassium dihydrogen phosphate pH 3.3, methanol, and acetonitrile mobile phases. The PDA detector was operated at 210 nm for TMZ and 225 nm for ATN and the flow rate was 1.0 mL/ min. Linearity was obtained over a concentration range of (1.0-100 μg/mL) for both analytes in standard solutions and the method was successfully applied for determination of target analytes in their pharmaceutical tablets. Excellent linearity was also obtained over concentration ranges of (0.25-25 μg/mL) and (0.5-25 μg/mL) in human urine for TMZ and ATN, respectively. A simple liquid-liquid extraction was applied for urine sample clean-up and a gradient method was used for chromatographic separation. The lower limit of quantitation (LOQ) was 0.99 and 0.60 μg/mL for ATN and TMZ, respectively. The limit of detection (LOD) was 0.30 and 0.18 μg/mL for ATN and TMZ, respectively. Inter- and intraday precision and accuracy for ATN were within ±1.89% in pure form and within ±2.85% in urine samples. Inter- and intraday precision and accuracy for TMZ were within ± 3.99% in pure form and within ± 3.19% in urine samples.

scholarly journals Validasi Metode Penentuan Benzena, Toluena dan Xilena pada Sampel Udara dan Tanah Menggunakan Kromatografi Gas

2019 ◽  
Vol 15 (1) ◽  
pp. 177
Author(s):  
Aman Sentosa Panggabean ◽  
Tika Widyastuti ◽  
Noor Hindryawati
Keyword(s):  
Gas Chromatography ◽  
Retention Time ◽  
Limit Of Detection ◽  
Soil Samples ◽  
Analytical Performance ◽  
Air Samples ◽  
Limit Of Quantitation ◽  
Benzene Toluene ◽  
Precision And Accuracy

<p>Penelitian tentang validasi metode penentuan kadar benzena, toluena dan xilena pada sampel udara dan tanah dengan menggunakan kromatografi gas telah dilakukan. Untuk mendapatkan hasil pengukuran yang valid, beberapa parameter penting yang berpengaruh dalam validasi metode telah ditentukan. Beberapa parameter penting yang dilakukan adalah penentuan besaran dasar kromatografi yang meliputi: waktu retensi, kapasitas (k’), faktor selektivitas (α) dan kinerja analitik yang meliputi: penentuan linearitas (r), limit deteksi (LOD), limit kuantitasi (LOQ), presisi dan akurasi. Hasil penelitian penentuan kinerja analitik sangat baik ditunjukkan oleh nilai presisi sebagai % KV &lt; 2/3 nilai KV Horwitz, LOD untuk masing-masing senyawa benzena, toluena dan xilena adalah 0,02 mg/L; 0,59 mg/L dan 0,08 mg/L serta LOQ untuk masing-masing senyawa benzena, toluena dan xilena adalah 0,07 mg/L; 1,99 mg/L dan 0,27 mg/L. Akurasi  metode ini sangat baik ditunjukkan dengan nilai presentase perolehan kembali masing-masing senyawa benzena, toluena dan xilena untuk sampel tanah sebesar 102,61 ± 4,61%; 101,65 ± 7,41%; 102,15 ± 4,15%, dan untuk sampel udara masing-masing senyawa sebesar 101,69 ± 5,77%; 102,08 ± 5,43% dan 98,55 ± 5,11%. Berdasarkan hasil penelitian ini, metode kromatografi gas dapat digunakan dalam penentuan benzena, toluena dan xilena pada sampel udara dan tanah dengan memberikan hasil yang valid.</p><p><strong>Validation Method </strong><strong>o</strong><strong>n The Determination </strong><strong>o</strong><strong>f Benzene, Toluene </strong><strong>a</strong><strong>nd Xylene </strong><strong>i</strong><strong>n Air </strong><strong>a</strong><strong>nd Soil Samples Using Gas Chromatography. </strong>The present study investigated the method for the determination of the content of benzene, toluene, and xylene in air and soil samples using gas chromatography. To obtain a valid measurement result, several important parameters that influence the method validation have been determined. The several important parameters carried out are the determination of the basic chromatographic such as retention time, capacity factor (k'), selectivity (α) and analytical performance measurement includes: the determination of linearity (r), limit of detection (LOD), limit of quantitation (LOQ), precision and accuracy. The result of analytical performance of the research are well verified, in which the value of precision was % CV &lt; 2/3 CV Horwitz value, LOD for benzene, toluene, and xylene compound were 0.02 mg/L, 0.59 mg/L, 0.08 mg/L, respectively, and LOQ for benzene, toluene and xylene compounds was 0.07 mg/L, 1.99 mg/L and 0.27 mg/L respectively. This method achieved high accuration, indicated by a percentage of recovery value of benzene, toluene, and xylene for soil samples of 102.61 ± 4.61%; 101.65 ± 7.41%; 102.15 ± 4.15%, and for air samples was 101.69 ± 5.77%, 102.08 ± 5.43%, and 98.55 ± 5.11% respectively. Based on the results of this research, the method presented in this study can be applied for the determination of benzene, toluene, and xylene using gas chromatography in air and soil samples with valid results.</p>

scholarly journals Development and Validation of New RP-HPLC Method for Simultaneous Determination of Methyl and Propyl Parabens with Levetiracetam in Pure Form and Pharmaceutical Formulation

2016 ◽  
Vol 2016 ◽  
pp. 1-5 ◽  
Author(s):  
Soad S. Abd El-Hay ◽  
Mostafa S. Mohram
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Gradient Elution ◽  
Hplc Method ◽  
Pure Form ◽  
Mobile Phase Flow Rate ◽  
Column Temperature ◽  
Limit Of Quantitation

A simple and robust high-performance liquid chromatography (HPLC) method is described for the assay for levetiracetam (LTC), methyl paraben (MHB), and propyl paraben (PHB) either in their pure form or in commercial Levepsy® syrup. The method is selective and stability indicating and all chromatographic conditions were studied to obtain adequate separation of LTC, MHB, and PHB from their degradation products and from excipients. The HPLC separation was carried out on a RP C18 Hypersil BDS analytical column (150 mm × 4.6 mm ID) using gradient elution system. The mobile phase flow rate was 1.5 mLmin−1 and the column temperature was kept at 40°C. Complete separation of the studied components was obtained within a cycle time of 8 min. LTC, MHB, and PHB were eluted at 1.56, 5.86, and 7.85 min, respectively. Detection was carried out at 240 nm using a dual wavelength detector. The method has been validated for linearity, accuracy, precision, specificity, limit of detection, limit of quantitation, robustness, and ruggedness. The proposed method was successfully applied for the determination of LTC in the presence of parabens in Levepsy syrup.

scholarly journals Determination of Nicotine in Libyan Smokers' Urine Compared with that of Nonsmokers using Reversed Phase – High Performance Liquid Chromatog-raphy (RP-HPLC)

2019 ◽  
Vol 34 (3) ◽  
pp. 172-180
Author(s):  
Galal Elmanfe ◽  
Suad K. Omar ◽  
Noreldin S.Y. Abdolla ◽  
Amna M. Hassan
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Cost Effective ◽  
High Performance Liquid Chromatog ◽  
Reversed Phase ◽  
Urine Samples ◽  
Average Value ◽  
Limit Of Quantitation ◽  
One Step

The aim of the present study was to evaluate the levels of nicotine in twenty urine samples taken from ten smokers and ten non-smokers in Libya. Each volunteer was required to complete a questionnaire before providing the urine sample. The evaluation of the nicotine concentrations was carried out by means of a simple, rapid, cost effective but reliable, one-step extraction technique-reversed-phase high-performance liquid chromatography which was developed and validated for this purpose. The criteria and factors taken into consideration for this evaluation and validation include the linearity, precision, accuracy, limit of detection, and limit of quantitation. The urine samples from the smokers presented nicotine concentrations in the range of 0.037-1.979 µg/ml, with an average of 0.663 µg/ml. The range of the nicotine concentrations in non-smokers, on the other hand, was from 0.017-1.331 g/ml, where 0.273 µg/ml is the average value. Statistical analyses show that the nicotine concentrations were very significant in the smoker samples in contrast with the nonsmoker samples

Development of Dispersive Liquid-Liquid Microextraction Procedure for Trace Determination of Malathion Pesticide in Urine Samples

2020 ◽  
Author(s):  
Maryam RAMIN ◽  
Monireh KHADEM ◽  
Fariborz OMIDI ◽  
Mehran POURHOSEIN ◽  
Farideh GOLBABAEI ◽  
...  
Keyword(s):  
Enrichment Factor ◽  
Human Urine ◽  
High Performance ◽  
Limit Of Detection ◽  
Urine Samples ◽  
Human Urine Samples ◽  
Extraction Solvent ◽  
Ultraviolet Detector ◽  
Relative Standard

Background: Measurement of pesticides in biological matrices is become a serious challenge for researches because of their very low concentration in different matrices. The aim of this study was to develop a new sample preparation method with high accuracy and validity, simplicity and short retention time for determination of malathion. Methods: Dispersive liquid-liquid micro-extraction (DLLME) technique coupled with high-performance liquid chromatography equipped with ultraviolet detector (HPLC-UV) developed for trace extraction and determination of malathion pesticide in human urine samples. This study was done in 2017 at Tehran University of Medical Sciences, Tehran, Iran. One variable at a time (OVAT) method was used to optimize parameters affecting the malathion extraction. Different parameters such as extraction solvent, disperser solvent, and volume of the extraction solvent, volume of the disperser solvent, centrifugation time and speed, salt addition, and sample pH were studied and optimized. Results: Under the optimized conditions, the limit of detection and enrichment factor of the method were 0.5 µg L-1 and 200, respectively. The calibration curve was linear in the concentration range of 2-250 µg L-1 . The relative standard deviation for six replicate experiments at 200 µg L-1 concentration was less than 3%. The relative recoveries of spiked urine samples were 96.3%, 101.7% and 97.3% at three different concentration levels of 50, 200 and 1000 µg L-1 , respectively. Conclusion: DLLME procedure was successfully developed for the extraction of malathion from human urine samples. Compared to other extraction techniques, the proposed procedure had some advantages such as shorter extraction time, better reproducibility, and higher enrichment factor.  

Capillary Electrophoresis Method for Determination of Escitalopram Oxalate in Urine Samples and Different Dosage Forms

2020 ◽  
Vol 58 (8) ◽  
pp. 759-769
Author(s):  
Wafa F S Badulla ◽  
Arın G Dal Poçan ◽  
Zeki Atkoşar ◽  
Göksel Arlı
Keyword(s):  
Capillary Electrophoresis ◽  
Limit Of Detection ◽  
Background Electrolyte ◽  
Dosage Forms ◽  
Fused Silica ◽  
Urine Samples ◽  
Effective Length ◽  
Simple Liquid ◽  
Pharmaceutical Dosage Forms

Abstract Application of capillary electrophoresis (CE) has become a rapidly growing analytical technique for the estimation of drugs in pharmaceutical dosage forms and biological fluids. In this study, an effective and sensitive method was developed for the determination of escitalopram oxalate (ESC-OX) by CE with diode-array detection at 200 nm. The separation was achieved by a fused silica capillary with 40 cm effective length (48.5 cm total, 75 μm i.d.). The background electrolyte was composed of 15 mM phosphate buffer (pH 2.5). The applied potential was 22.5 kV, and the samples were injected at 50 mbar pressure for 10 s. Metoprolol was used as an internal standard (IS). The migration time under these optimum conditions was 6.51 ± 0.07 and 6.73 ± 0.08 min for ESC-OX and IS, respectively, with total run time 7 min. The method was validated for linearity, precision, accuracy, specificity and sensitivity. The limit of detection was calculated as 3.85 and 5.07 ng mL−1 for standard and urine samples, respectively. The developed method was employed successfully for the determination of ESC-OX in different pharmaceutical dosage forms and spiked human urine after simple liquid–liquid extraction with good recovery.

Spectrophotometric Determination of Zolmitriptan in Pure Form and in Tablets Through Charge Transfer Complex Reaction

2019 ◽  
Author(s):  
Safwan Ashour
Keyword(s):  
Charge Transfer ◽  
Limit Of Detection ◽  
Pharmaceutical Preparations ◽  
Dominant Mode ◽  
Pure Form ◽  
Apert Syndrome ◽  
Charge Transfer Complexes ◽  
Midfacial Hypoplasia ◽  
Limit Of Quantitation

Apert syndrome (AS) a type of acrocephalosyndactyly is a rare congenital disorder with autosomal dominant mode of transmission that consists of craniofacial synostosis, midfacial hypoplasia and bilateral limb syndactyly. Patients present in early childhood for multiple surgeries which make it imperative to know about various anaesthetic implications like difficult airway ventilation, airway hyper reactivity, associated congenital anomalies, increased airway secretions and deranged temperature thermoregulation associated with this syndrome. The patient should be thoroughly evaluated preoperatively and managed accordingly. We discuss the successful management of a three and a half years old male child two simple, rapid and selective colorimetric methods were developed for the determination of zolmitriptan (ZMT) in pure form and pharmaceutical preparations. These methods are based on the directly formation of charge-transfer complexes between ZMT and m-nitrophenol (MNP) in aqueous medium (ZMT: MNP, 1:1) and 2,4-dinitrophenol (DNP) in ethanol:water (80:20). The developed method involves formation of coloured complexes (1:1) of ZMT with MNP and DNP. The yellow formed complexes were quantitatively measured at 400 and 440 nm for ZMT-MNP and ZMT-DNP, respectively. Beer's law was obeyed in the concentration ranges of 3.0–260 μg/mL for MNP and 3.5–120 μg/mL for DNP. Limit of detection and limit of quantitation for MNP were calculated as 0.58 and 1.75 μg/mL, respectively, and for DNP were 0.32 and 0.97 μg/mL, respectively. The method was validated with respect to accuracy, robustness and selectivity. The proposed method has been successfully applied for the determination of ZMT in tablets.

scholarly journals Quantitative determination of major nandrolone metabolite in human urine by gas chromatography/mass spectrometry

2019 ◽  
pp. 78-85
Author(s):  
Pavel G. Shahoika ◽  
Aliaksandr A. Ahabalayeu ◽  
Olga N. Tchekhovskaya ◽  
Yury G. Pakhadnia ◽  
Sergey A. Beliaev ◽  
...  
Keyword(s):  
Quantitative Determination ◽  
Human Urine ◽  
Internal Standard ◽  
Urine Samples ◽  
Gas Chromatography Mass Spectrometry ◽  
Liquid Liquid Extraction ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
World Anti Doping Agency

Nandrolone is an anabolic androgenic steroid. The use of this substance is prohibited by World Anti-Doping Agency (WADA). In National Anti-Doping Laboratory, we have developed method for quantitative determination of major nandrolone metabolite – 19-norandrosterone in human urine by GC/MS technique (Agilent 7000). Proposed method includes sample preparation of urine samples with enzymatic hydrolysis, liquid-liquid extraction followed by derivatization step with MSTFA. Deuterated 19-norandrosterone has been used as internal standard. Total run time comprised 16 min. Lower limit of quantitation accounted for 1 ng/mL. Spiked urine samples were prepared by mixing blank urine with standard solutions of 19-norandrosterone in range 1–30 ng/mL, correlation coefficient larger than 0.99. Method was verified to following validation parameters: selectivity, linearity, repeatability, accuracy, matrix effect, stability and robustness. Furthermore, measurement uncertainty was estimated. Thus, proposed method is able to detect threshold 19-norandrosterone in human urine and carry out its quantitation conforming WADA requirements.

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