scholarly journals Simultaneous spectrophotometric determination of phenanthridine, phenanthridinone and phenanthridine N-oxide using multivariate calibration methods

2010 ◽  
Vol 8 (1) ◽  
pp. 207-213 ◽  
Author(s):  
Mohammad-Hossein Sorouraddin ◽  
Kaveh Amini ◽  
Abdolhossein Naseri ◽  
Mohammad-Reza Rashidi

AbstractThe multivariate calibration methods, partial least squares (PLS) and principle component regression (PCR) have been used to determine phenanthridine, phenanthridinone and phenanthridine N-oxide in spiked human plasma samples. Resolution of binary and ternary mixtures of analytes with minimum sample pre-treatment and without analyte separation has been successfully achieved analyzing the UV spectral data. The net analyte signal (NAS) concept was also used to calculate multivariate analytical figures of merit such as limit of detection, selectivity and sensitivity. The simultaneous determination of three analytes was possible by PLS and PCR processing of sample absorbance in the 210–355 nm region. Good recoveries were obtained for both synthetic mixtures and spiked human plasma samples.

2005 ◽  
Vol 88 (2) ◽  
pp. 455-461 ◽  
Author(s):  
Mohamed A El Dawy ◽  
Mokhtar M Mabrouk ◽  
Riad A El Barbary

Abstract A spectrofluorimetric method is described for the determination of drugs containing active methylene groups adjacent to carbonyl groups. The method was applied successfully to the determination of warfarin sodium in laboratory-prepared mixtures, in commercial tablets, and in spiked human plasma samples. Finally, the method was applied to the determination of the steady-state concentration of warfarin sodium in the blood of a hospitalized patient. The method involves the reaction of warfarin sodium with 0.2 ml (0.4 × 10−3M) N1-methylnicotinamide chloride reagent in the presence of 3 mL 1.0N NaOH and cooling in ice for 8 min, followed by adjustment of the pH to 2.0, using formic acid and heating for 4 min, whereby a highly fluorescent reaction product is produced. The optimal wavelengths of excitation and emission were determined by using a synchronous wavelength search and found to be 284 and 354 nm, respectively. The standard curves were linear over a concentration range of 50–1500 ng/mL in both aqueous solutions and spiked human plasma samples. The mean recoveries (± standard deviation) were 101.157 (±1.33) and 95.73 (±1.88%) for aqueous solutions and spiked human plasma samples, respectively. The method showed good specificity and precision. The proposed method is simple and economical because of its minimal instrumentation and chemicals requirements. Nevertheless, it is highly sensitive, specific, and reproducible. Accordingly, it is suitable for quality-control applications, drug monitoring, and bioavailability and bioequivalency studies.


2012 ◽  
Vol 2012 ◽  
pp. 1-13
Author(s):  
Khaled M. Elokely ◽  
Mohamed A. Eldawy ◽  
Mohamed A. Elkersh ◽  
Tarek F. El-Moselhy

A simple fluorometric method, using -methylnicotinamide chloride (NMNCl) as a fluorogenic reagent, has been developed, adapted, and validated for the quantitative estimation of drugs containing α-methylene sulfoxide functional groups. The proposed method has been applied successfully to the determination of sulindac (1), omeprazole (2), lansoprazole (3), pantoprazole (4), and rabeprazole (5) in the pure form, laboratory-prepared mixtures, pharmaceutical dosage forms, spiked human plasma samples, and in hospitalized patient's or volunteer's blood. For the standard solutions of 1, 2, 3, 4, and 5, the method showed linearity over concentration ranging between 1–50 g/mL, 50–1200 ng/mL, 100–1500 ng/mL, 10–1500 ng/mL, and 20–2200 ng/mL, respectively. For the spiked human plasma of 1, 2, 3, 4, and 5, the linearity was shown over concentration ranging between 1–50 μg/mL, 75–1200 ng/mL, 100–1400 ng/mL, 10–1500 ng/mL, and 50–2100 ng/mL, respectively. The method showed good accuracy, specificity, and precision in both laboratory-prepared mixtures and spiked human plasma samples. The proposed method is simple, does not need sophisticated instrumentation, suitable for quality control application, bioavailability, and bioequivalency studies. Besides, the sensitivity and detection limits are comparable to sophisticated chromatographic methods.


2020 ◽  
Vol 16 ◽  
Author(s):  
Paria Habibollahi ◽  
Azam Samadi ◽  
Alireza Garjani ◽  
Samad Shams Vahdati ◽  
Hamid-Reza Sargazi ◽  
...  

BACKGROUND: Tramadol, (±)-trans-2-[(dimethylamino) methyl]-1-(3-methoxyphenyl) cyclohexanol, is a synthetic centrally acting analgesic used in the treatment of moderate to chronic pain. Tramadol like other narcotic drugs is used for the treatment of pain and also may be abused. Its overdose can cause adverse effects such as dizziness, vomiting, and nausea. The aim of this paper is to develop a sample preparation method for the determination of tramadol in human plasma samples followed by CE analysis. METHODS: Ultrasound assisted-dispersive liquid–liquid microextraction using binary mixed extractant solvent (chloroform and ethyl acetate) was used for extraction of one hundred microliters of tramadol spiked human plasma samples and in real human plasma samples obtained from the patients with abuse of tramadol. After evaporation the extractant solvent, the residue was reconstituted in 100 µL deionized water and subsequently analyzed by CE-UV. RESULTS: The developed method has remarkable characteristics including simplicity, good repeatability and appreciable accuracy. Under the best extraction conditions, low limit of detection at 7.0 µg per liter level with good linearity in the range of 0.02–10 µg mL‒1 was obtained. CONCLUSION: UA-DLLME using a binary mixed extraction solvent was established for the determination of tramadol in human plasma samples via CE method with UV-detection. In addition, the analysis of tramadol in some plasma samples of patients with abuse of tramadol indicated that the method has acceptable performance for determination of tramadol in plasma samples which indicate that the method is suitable for clinical applications.


2011 ◽  
Vol 2011 ◽  
pp. 1-9 ◽  
Author(s):  
Khaled M. Elokely ◽  
Mohamed A. Eldawy ◽  
Mohamed A. Elkersh ◽  
Tarek F. El-Moselhy

A simple spectrofluorometric method has been developed, adapted, and validated for the quantitative estimation of drugs containing -methylene sulfone/sulfonamide functional groups usingN1-methylnicotinamide chloride (NMNCl) as fluorogenic agent. The proposed method has been applied successfully to the determination of methyl sulfonyl methane (MSM)(1), tinidazole(2), rofecoxib(3), and nimesulide(4)in pure forms, laboratory-prepared mixtures, pharmaceutical dosage forms, spiked human plasma samples, and in volunteer's blood. The method showed linearity over concentration ranging from 1 to 150 g/mL, 10 to 1000 ng/mL, 1 to 1800 ng/mL, and 30 to 2100 ng/mL for standard solutions of1,2,3, and4, respectively, and over concentration ranging from 5 to 150 g/mL, 10 to 1000 ng/mL, 10 to 1700 ng/mL, and 30 to 2350 ng/mL in spiked human plasma samples of1,2,3, and4, respectively. The method showed good accuracy, specificity, and precision in both laboratory-prepared mixtures and in spiked human plasma samples. The proposed method is simple, does not need sophisticated instruments, and is suitable for quality control application, bioavailability, and bioequivalency studies. Besides, its detection limits are comparable to other sophisticated chromatographic methods.


2006 ◽  
Vol 29 (15) ◽  
pp. 2265-2283 ◽  
Author(s):  
Gorka Iriarte ◽  
Nerea Ferreirós ◽  
Izaskun Ibarrondo ◽  
Rosa Maria Alonso ◽  
Miren Itxaso Maguregi ◽  
...  

2012 ◽  
Vol 38 (02) ◽  
pp. 178-184 ◽  
Author(s):  
Job Harenberg ◽  
Sandra Erdle ◽  
Svetlana Marx ◽  
Roland Krämer

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