scholarly journals Simultaneous determination of compounds in Septalen® pellets by derivative spectrophotometry

2000 ◽  
Vol 65 (5-6) ◽  
pp. 339-344 ◽  
Author(s):  
Mirjana Medenica ◽  
Darko Ivanovic ◽  
Andjelija Malenovic

In this paper, a second-derivative spectrophotometric method of assaying Septalen ? pellets (Krka, Novo Mesto, Slovenia), which contain lidocaine 1 mg, and cetrimoniumbromide 2mg, is described. Lidocaine, 2-(diethylamino)-N-(2,6-dimethyl- phenyl)-acetamide, is a local anesthetic with pronounced antiarhythmic and anticonvulsant properties. Cetrimoniumbromide, N,N,N-trimethyl-l-hexadecanaminium bromide, is a topical antiseptic and cleansing agent. Lidocaine was determined at 250 nm using the "zero crossing" technique because the signals of centrimonium bromide and the colour ingredient are zero at this wavelength. Cetrimonium bromide was determined by correction of the peak amplitude at 215 nm according to lidocaine. In choosing the optimal magnitudes for the simultaneous determination of both drugs, the following criteria were considered: (1) the linearity of the calibration graphs as given by the correlation coefficients, (2) the intercept, (3) the sensitivity as given by the regression coefficient, (4) the degree of interference in the derivative measurement by the presence of the other compound, as given by the relative percent error and by the relative recovery, and (5) the reproducibility, as given by the coefficient of variation, calculated by recording the second-derivative spectra.

1997 ◽  
Vol 80 (2) ◽  
pp. 325-330 ◽  
Author(s):  
Challapalli V N Prasad ◽  
Vipin Bharadwaj ◽  
Vidya Narsimhan ◽  
Rama T Chowdhary ◽  
Pyare Parimoo

Abstract A derivative spectrophotometric procedure was established for simultaneous determination of propranolol HCI (PP) with hydrochlorothiazide (HTZ) and metoprolol tartrate (MTP) with HTZ in tablet preparations. The method uses first- and second-derivative spectra of tablet extract in 0.01 N NaOH solution. Ratios of analyte concentrations in the mixture were determined by the compensation technique. The zero-crossing point (ZCP) was also used to estimate the amounts of PP and HTZ in the formulations, and results were compared with those from the compensation technique. The results were found to be precise and free from interferences.


1988 ◽  
Vol 34 (6) ◽  
pp. 1119-1121 ◽  
Author(s):  
B Dingeon ◽  
M A Charvin ◽  
M T Quenard ◽  
H Thome

Abstract Measurement of acetaminophen by analysis of the second derivative of its spectrum is specific and sensitive. The method of extraction and the use of just one phosphate buffer as reagent makes this method very convenient. Readings are reliable from 10 to 1500 mg/L. A turnaround time of 20 min makes this method well suited for emergency cases. Precision and accuracy of the method are presented. Results are not biased by interferences, not even from N-acetylcysteine.


2017 ◽  
Vol 100 (1) ◽  
pp. 38-44
Author(s):  
Kunjan Bodiwala ◽  
Shailesh Shah ◽  
Yogini Patel ◽  
Pintu Prajapati ◽  
Bhavin Marolia ◽  
...  

Abstract Two sensitive, accurate, and precise spectrophotometric methods have been developed and validated for the simultaneous estimation of ofloxacin (OFX), clotrimazole (CLZ), and lignocaine hydrochloride (LGN) in their combined dosage form (ear drops) without prior separation. The derivative ratio spectra method (method 1) includes the measurement of OFX and CLZ at zero-crossing points (ZCPs) of each other obtained from the ratio derivative spectra using standard LGN as a divisor, whereas the measurement of LGN at the ZCP of CLZ is obtained from the ratio derivative spectra using standard OFX as a divisor. The double divisor-ratio derivative method (method 2) includes the measurement of each drug at its amplitude in the double divisor-ratio spectra obtained using a standard mixture of the other two drugs as the divisor. Both methods were found to be linear (correlation coefficients of >0.996) over the ranges of 3–15, 10–50, and 20–100 μg/mL for OFX, CLZ, and LGN, respectively; precise (RSD of <2%); and accurate (recovery of >98%) for the estimation of each drug. The developed methods were successfully applied for the estimation of these drugs in a marketed ear-drop formulation. Excipients and other ingredients did not interfere with the estimation of these drugs. Both methods were statistically compared using the t-test.


2002 ◽  
Vol 85 (4) ◽  
pp. 883-888 ◽  
Author(s):  
M Inés Toral ◽  
César Soto ◽  
Pablo Richter ◽  
Ana E Tapai

Abstract This paper reports a simple and fast method for the simultaneous determination of estradiol (ED) and medroxyprogesterone acetate (MP) in pharmaceutical formulations by second-derivative spectrophotometry. Methanol was used to extract the drugs from formulations, and subsequently the extracts were evaluated directly by derivative spectrophotometry. The drugs were determined simultaneously by using the graphic method at 297.4 nm for ED and the zero-crossing method at 273.4 nm for MP. If both compounds are present together in a sample, it is possible to quantitate one in the presence of the other. The best signal-to-noise ratio was found when the second derivative of the spectrum was used. The linear ranges for determination of the drugs were 4.7 × 10−6 to 1.6 × 10−4 and 7.2 × 10−6 to 2.0 × 10−4 mol/L for ED and MP, respectively. The ingredients commonly found in commercial pharmaceutical formulations do not interfere with the determination. Chemical and spectral variables were optimized for the determination of both analytes. Good levels of repeatability (relative standard deviation), 1.4 and 1.9%, were obtained for ED and MP, respectively. The proposed method was applied to the determination of these drugs in pharmaceutical formulations.


1995 ◽  
Vol 3 (4) ◽  
pp. 219-225 ◽  
Author(s):  
Hitoshi Takamura ◽  
Noriko Hyakumoto ◽  
Naoko Endo ◽  
Teruyoshi Matoba ◽  
Tamako Nishiike

The relationship between near infrared (NIR) second derivative spectra and lipid oxidation was investigated to develop a method for the determination of lipid oxidation in edible oils by NIR spectroscopy, using peroxide value ( POV) as the index of oxidation. Although several absorption peaks were found in the difference second derivative spectra of oxidised edible oils, the intensity of the peak at 2084 nm only was highly correlated to POV. In the spectra of purified hydroperoxides of methyl oleate and methyl linoleate, the intensity of the peak at 2084 nm was also highly correlated with POV, which demonstrates that the absorption is due to hydroperoxide. In addition, this peak shifted and weakened after reduction of hydroperoxide to hydroxide, which shows the absorption is specific for the hydroperoxyl group. These results suggest that 2084 nm is the key wavelength for lipid peroxide and can be used for the determination of lipid oxidation in edible oils.


2004 ◽  
Vol 87 (6) ◽  
pp. 1323-1328 ◽  
Author(s):  
M Inés Toral ◽  
Maximiliano Paine ◽  
Patricio Leyton ◽  
Pablo Richter

Abstract A new method for the sequential determination of attapulgite and nifuroxazide in pharmaceutical formulations by first-and second-derivative spectrophotometry, respectively, has been developed. In order to obtain the optimal conditions for nifuroxazide stability, studies of solvent, light, and temperature effects were performed. The results show that a previous hydrolysis of 2 h in 1.0 × 10–1M NaOH solution is necessary in order to obtain stable compounds for analytical purposes. Subsequently, the first-and second-derivative spectra were evaluated directly in the same samples. The sequential determination of the drugs can be performed using the zero-crossing method; the attapulgite determination was carried out using the first derivative at 278.0 nm and the nifuroxazide determination, using the second derivative at 282.0 nm. The determination ranges were 5.7 × 10–6–1.0 × 10–4 and 3.7 × 10–8 –1.2 × 10–4M for attapulgite and nifuroxazide, respectively. Repeatability (relative standard deviation) values of 1.2 and 3.0% were observed for attapulgite and nifuroxazide, respectively. The ingredients commonly found in commercial pharmaceutical formulations do not interfere. The proposed method was applied to the determination of these drugs in tablets. Further, infrared spectroscopy and cyclic voltammetry studies were carried out in order to obtain knowledge of the decomposition products of nifuroxazide.


2019 ◽  
Vol 9 (2) ◽  
pp. 25-29
Author(s):  
Muharram Y. Mohammad ◽  
Mohammad S. Abdullah ◽  
Sangar S. Sabir

The present study describes employing second derivative spectrophotometry for simultaneous determination of atenolol and amlodipine in pure form and in commercial formulations. The method is simple, accurate, precise and economic. Zero crossing point technique was used for analysis of the drugs in the combined formulation. The method was found to be linear in the concentration range 5.0-50.0µg/ml of atenolol at 251nm and 5.0-45.0µg/ml of amlodipine at 264nm. The proposed method was successfully applied to determine atenolol and amlodipine in combined dosage as well as in a separate dosage. The obtained results were in good agreement with standard method.  


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