Derivative Spectrophotometric Method Research Articles

Derivative Spectrophotometric Methods for Simultaneous Determination of Quercetin and Gentisic acid in Capparis spinosa L.

الشفلح هو أحدی النباتات الطبية الذي یستخدم في الطب التقليدي و یتضمن المواد الكيميائية النباتية العديدة مثل المركبات بوليفينولیة. تعتبر كلتا المركبتين، كویرستین وحامض الجینتسیك، کمركب فينولية مهمة اللتان توجدان في النباتات ولهما الخصائص الطبية الکثیرة مثل مضاد الالتهابات، مضاد الميكروبات، مضاد الأكسدة ومضاد للسرطان. لم يتم التحقق بعد من تحديد كلا المركبين معًا في مزیج ثنائي باستخدام طرق القياس الطيفي. في هذه الدراسة، تم تطوير طريقتين طيفيتين مشتقتين بسيطتين سريعتين و دقيقتين لاستخدامهما للتقدير الكمي الآنی لمادة كویرستین وحامض الجینتسیك في المزيج الثنائية وخلاصة أوراق الشفلح. الطريقة الأولی تعتمد على استخدام طریق العبور الصفري (المشتق الأول والرابع) ، بينما الطريقة الثانية هي المشتق الأول لأطياف النسبة. الخطية لمنحنيات المعايرة لكلتا الطريقتين الطيفية المشتقة يتراوح تركيزهما بين 2.0-30 ميكروغرام / مل و 4.0-80 ميكروغرام / مل لكویرستین وحامض الجینتسیك، على التوالي، في حين تراوحت نسب الاسترداد من 94.06٪ الی 105.98٪ (كویرستین) و 94.29٪ الی 113.37٪ (حمض الجینتسیك). تم استخدام الطرق المطورة بشكل فعال في التقدیر الكمي لكل من المركبات الفينولية في أوراق الشفلح..

Simultaneous biosorption of acid violet and reactive yellow dyes by Cladosporium cladosporioides

AbstractThe synthetic dye mixture of Acid Violet 90 and Reactive Yellow 145 was treated with dead Cladosporium cladosporioides biomass. The individual concentrations were calculated with the first-order derivative spectrophotometric method. The calibration curves were plotted at wavelengths of 578.4 nm and 318.2 nm in the derivative spectrum for Acid Violet 90 and Reactive Yellow 145, respectively. The calculated limit of quantitation value is ~ 2.5 mg/L for Acid Violet 90 and ~ 1.5 mg/L for Reactive Yellow 145. The achieved mean recovery percentage values are around 100%. The highest removal efficiency (100%) was obtained for both dyes at pH 4 using 0.25 g biomass and 50 mg/L of each dye in 60 min reaction time with 150 rpm shaking speed. The hydrochloric acid solution was used for biomass regeneration, and the removal efficiencies remained at 99% and 89% for Acid Violet 90 and Reactive Yellow 145 in the third cycle. Graphical abstract

Development and Validation of HPTLC and First Derivative Spectrophotometric Methods for Determination of Levetiracetam in Bulk and Tablet Dosage Form

A simple, sensitive high performance thin layer chromatographic (HPTLC) method and first order derivative spectrophotometric methods were developed for estimation of US FDA drug levetiracetam in bulk and its tablet dosage form. Chromatographic estimation was carried out on silica gel 60 F245 TLC plate as stationary phase and toluene: methanol: Ethyl acetate (4:4:2v/v/v) as mobile phase. Densitometric analysis was carried out at wavelength 218nm. The Rf values for Levetiracetam was found to be 0.47±0.03. Linearity was observed over range of 400-3200ng/spot for Levetiracetam (R2 0.998). The %recovery of Levetiracetam was found to be 99.25-100.7%. The LOD and LOQ were found to be 0.0917ng/ml and 0.278ng/ml respectively indicating sensitivity of the method. The first order derivative spectra were obtained at n=4, Δλ=3nm and determinations was made at 215 nm using methanol as solvent. Linearity was observed in the range of 80μg/ml - 280μg/ml with good regression values. Percent mean recovery of Levetiracetam was obtained as 101.5%. Both proposed methods were simple, fast, accurate, precise and reproducible and hence can be applied for routine quality control analysis of levetiracetam in bulk and its tablet dosage form.

First-order derivative spectrophotometric method for simultaneous determination of brinzolamide and timolol maleate in ophthalmic formulation

Multi-analyte determination techniques are favored over those that can only determine a single analyte at a time because they enable resource savings (cost, time, and solvents) and reduce generated waste and the number of samples required for analysis. This research presents a novel method for the simultaneous determination of brinzolamide (BRZ) and timolol maleate (TML) in pharmaceutical ophthalmic preparations using first-order derivative UV–Visible spectroscopy. The proposed approach is environmentally friendly and yet to be previously reported in the literature. In this approach, the peak amplitude of BRZ was quantified at the zero-crossing point of TML, i.e., 248.80 nm, whereas TML was determined by measuring absorbance at 297.60 nm. The developed method was validated according to the International Council for Harmonisation guidelines Q2(R1). The developed method was linear with excellent correlation coefficient values (R2 > 0.9998) in the range of 4 – 24 µg/ml for BRZ and 5 – 25 µg/ml for TML. The accuracy and precision results were within limits for both the analytes (%Relative standard deviation, RSD <2 %). The proposed method demonstrated LOD = 0.38 µg/mL for BRZ and 0.98 µg/mL for TML; LOQ = 0.91 µg/mL for BRZ and 2.99 µg/mL for TML), and was found to be selective, and robust. Lastly, the novel Analytical GREEnness (AGREE) metrics, the analytical eco-scale, and the green analytical procedure index (GAPI) were utilized to evaluate the developed technique's environmental sustainability and compare it to the HPLC method.

Derivative spectroscopy and wavelet transform as green spectrophotometric methods for abacavir and lamivudine measurement

Herein, two different sustainable and green signal processing spectrophotometric approaches, namely, derivative spectroscopy and wavelet transform, have been utilized for effective measurement of the antiretroviral therapy abacavir and lamivudine in their pharmaceutical formulations. These methods were used to enhance the spectral data and differentiate between the absorption bands of abacavir and lamivudine in order to accurately measure their concentrations. For determining abacavir and lamivudine, the first derivative spectrophotometric method has been applied to the zero-order and ratio spectra of both drugs. The same approach has been tested using the continuous wavelet transform method where a second order 2.4 of rbio and bior wavelet families were found to be optimum for measuring both drugs. Validation of the proposed methods affirmed their reliability in terms of linearity over the concentration range 1.5–30 µg/mL and 1.5–36 µg/mL for abacavir and lamivudine, respectively, precision (RSD < 2 %), and accuracy with mean recoveries ranging between 98 % and 102 %. Additionally, these spectrophotometric methodologies were applied to real pharmaceutical preparations and yielded results congruent with a prior chromatographic method. Most prominently, the proposed methods stood out for their greenness and sustainability with 97 points as evaluated by the analytical eco-scale method and a score value of 0.79 as analyzed by AGREE method, thereby making them suitable for resource-limited settings and highlighting the potential for broader application of green analytical methods in pharmaceutical analysis.

Stability Indicating Derivative Spectrophotometric Method for Determination of Trandolapril in Bulk and in Formulation

Stability Indicating Derivative Spectrophotometric Method for Determination of Trandolapril in Bulk and in Formulation

Evaluation of Stability and TLC Fingerprinting of the Artemether Component in Artemether-Lumefantrine Combination Suspension Formulations Available in Nigeria Pharmaceutical Market

Aim: Artemether is the main component of the artemisinin-based combination therapy (ACT), used in the management of malaria infection caused by Plasmodium falciparum. Hence, its stability and conformation to pharmacopeia standards are necessary for use. The study aimed to review the first-order derivative spectrophotometric method for simultaneous estimation of artemether and its derivatives in pure and combined formulations, and their stability profiles, then develop a simple, precise, and fast technique for their rapid physicochemical analysis.&#x0D; Methodology: Thin-layer chromatographic (TLC) Fingerprinting principles were used in the analysis. Artemether and its derivatives were spotted on the TLC chromatograms after adding 25 mL of the suspension to a mixture of 100 mL of distilled water and 4 mL of NaOH, extracting the mixture with 60 mL of dichloromethane (DCM), drying, and sonicating the residue with 20 mL of the solvent. It was centrifuged, and the clear supernatant was spotted on the TLC plates.&#x0D; Results: The color test results revealed the presence of the artemether compound in the reference standard as well as the six brands of suspensions (A, B, C, D, E, and F) utilized in the study. Artemether melting point was obtained between 86 - 89 °C; within the International Pharmacopeia specified range. The chromatograms of Artemether and derivatives showed Rf values of 0.25 (impurity A), 0.3 (artenimol impurity B), 0.35 (impurity C), 0.4 (α-artemether: impurity D), and 0.55 (artemether).&#x0D; Conclusion: The devised method can be applied to the routine quality control analysis of artemether-lumefantrine suspension in addition to existing analytical techniques.

Validated Simultaneous Derivative Spectrophotometric Estimation of Azithromycin, Fluconazole and Secnidazole in Bulk and Pharmaceutical Formulation

Two simple, sensitive, accurate and precise spectrophotometric methods were developed and validated for the quantitative determination of Azithromycin (AZI), Fluconazole (FLU) and Secnidazole (SEC) in bulk and tablet dosage form. Method A is based on the first-order derivative (D1) and Method B is based on the second-order derivative (D2) spectrophotometric method. In Method A, absorbance was measured at 215nm, 275nm and 333nm being the zero crossing points for AZI, FLU and SEC respectively. In Method B, absorbance was measured at 220nm, 225nm and 211nm being the zero crossing points for AZI, FLU and SEC respectively. For Method A, all three drugs obey Beer’s law in the concentration range 5-30µg/ml for AZI, 5-60 µg/ml for FLU and 5-40 µg/ml for SEC with correlation coefficients 0.995, 0.998 and 0.998 respectively. For Method B, all three drugs obey Beer’s law in the concentration range 5-35 µg/ml for AZI, 5-40 µg/ml for FLU and 5-40 µg/ml for SEC with correlation coefficients 0.995, 0.999 and 0.998 respectively. Both methods can be used for routine analysis of these three drugs in their pharmaceutical dosage form. Results for analysis of both methods were tested and validated for various parameters according to ICH guidelines. &#x0D; Keywords: Derivative, Azithromycin, Fluconazole, Secnidazole

Derivative Spectrophotometric method for Simultaneous Determination the residue of Carboxin, Chlorothalonil and Pyriproxyfen in cabbage samples using Zero-crossing Technique

Derivative Spectrophotometric method for Simultaneous Determination the residue of Carboxin, Chlorothalonil and Pyriproxyfen in cabbage samples using Zero-crossing Technique

Validated Analytical Method for Multicomponent Analysis of Famotidine and Ofloxacin in Bulk drug and Tablet Formulation by using UV-Visible Spectrophotometer and RP-HPLC

A simple, sensitive, accurate, precise, and reproducible UV- spectrophotometric method and RP-HPLC methods were developed and validated for the estimation of Famotidine and Ofloxacin in bulk drug and pharmaceutical formulation. The Linearity regression was detected and shows a good linear relationship; in the concentration range of 10-50µg/mL (R2 &gt;0.9908) for famotidine and 10-50µg/mL (r2&gt;0.9913) for ofloxacin. The UV – spectrophotometric estimation was carried out by the first-order derivative spectrophotometric method and absorbance were recorded at 273 and 280nm. Beers range were found to be 5-50µg/mL, respectively for both drugs while, correlation coefficient r2 &gt; 0.9988 and 0.9941 for famotidine and ofloxacin. The isoabsorptive point was found to be 274nm in HPLC optimized mobile phase composition, potassium dihydrogen orthophosphate: methanol (60:40). Chromatographic condition consisted of mobile phase potassium dihydrogen orthophosphate buffer pH 2.3, methanol (60:40v/v), run time 30 min, C-18 column (ODS Hypersil) and flow rate 0.8mL/minute. The retention time for famotidine and ofloxacin were found to be 2.44 min, 7.99 min. respectively, and detection at λmax 274nm for both drugs (overlain spectra). The UV methods and RP-HPLC showed good reproducibility and recovery with the percent relative standard deviation (RSD) less than 5%. As per ICH guidelines, the developed method was validated for linearity, accuracy, precision, Sandell's sensitivity, and repeatability proving its utility in the estimation of famotidine and ofloxacin in house tablet formulation.

Stability Indicating Derivative Spectrophotometric Methods for Determination of Valbenazine Tosylate in Bulk and in Formulation

Stability Indicating Derivative Spectrophotometric Methods for Determination of Valbenazine Tosylate in Bulk and in Formulation

Validated Simultaneous Derivative Spectrophotometric Estimation of Diflunisal and Lignocaine in Bulk and Pharmaceutical Formulation

Two simple, sensitive, accurate and precise spectrophotometric methods were developed and validated for the quantitative determination of Diflunisal (DIF) and Lignocaine (LIG) in bulk and pharmaceutical dosage form. Method A is based on the first-order derivative (D1), and Method B is based on the second-order derivative (D2) spectrophotometric method. In Method A, absorbance was measured at 224nm and 264nm being the zero crossing points for DIF and LIG, respectively. In Method B, absorbance was measured at 232nm and 273nm being the zero crossing points for DIF and LIG, respectively. For Method A, the two drugs obeyed Beer's law in the concentration range of 3-39µg/ml for DIF and 4-40 µg/ml for LIG with correlation coefficients 0.999 and 0.995, respectively. For Method B, the two drugs obeyed Beer’s law in the concentration range of 3-30µg/ml for DIF and 4-48µg/ml for LIG with correlation coefficients 0.998 and 0.996, respectively. Both methods can be used for routine analysis of these two drugs in their pharmaceutical dosage form. Results for analysis of both methods were tested and validated for various parameters according to ICH guidelines. &#x0D; Keywords: Derivative, Diflunisal, Lignocaine, first order, second order

Development and Validation of Derivative UV Spectrophotometric method for Simultaneous Determination of Amoxicillin and Clavulanic acid in Tablets (Augmentin 1000mg)

The simultaneous analysis of pharmaceutical mixtures by classical spectrophotometric methods without prior separation is a challenge owing to the strong overlapping of their zero order spectra (low selectivity). Hence, several techniques have been developed for solving this problem, such as derivative spectrophotometry. The aim of this study was to develop a simple, fast, accurate, precise, economical, and eco-friendly derivative spectrophotometric method for the quantitative determination of a binary mixture of amoxicillin (Amox) and clavulanic acid (Clav) without prior separation steps. The developed method is based on the use of first derivative spectra resulting from derivatisation of zero order, with using these parameters (d𝛌=4 and scaling factor=15). The measurements were achieved by using zero-crossing technique (𝛌= 278.5nm for Amox and 𝛌= 228.3nm for Clav), which eliminated the overlapping caused by two drugs and excipients of tablets. The method showed significant linearity in the range (5 45μg/ml with =0.9998) and (1 - 10μg/ml with =0.9986) for Amox and Clav, respectively. The developed technique was validated according to the ICH guidelines. The method was successfully utilized for the simultaneous determination of Amox and Clav in the formulation. The obtained results were statistically compared with the reported method (HPLC) by applying t-test and F-value at 95% confidence level. No significant difference was observed regarding accuracy and precision. Hence,the proposed procedure can be utilized for regular quality control studies as alternative to chromatographic techniques.

Development &amp; determination of UV method for sildenafil &amp; fluxetine in bulk drug &amp; in formulation

A simple, rapid, precise and highly selective spectrophotometric method was developed for simultaneous estimation of Sildenafil citrate and Fluoxetine Hydrochloride in tablet dosage form. This method, involves the measurement of absorbances of Sildenafil citrate and Fluoxetine Hydrochloride at the wavelengths of 282nm (λmax of Sildenafil citrate) and 249 nm (λmax of Fluoxetine Hydrochloride). Methanol was used as solvent. Linearity was observed in the concentration range of 10-18µg/ml for Sildenafil citrate and 3-8ug/ml. Fluoxetine Hydrochloride. The accuracy of the method was confirmed by recovery studies of tablet dosage forms and was found to be 98.1% and 99.2% for Sildenafil citrate and Fluoxetine Hydrochloride respectively. The method showed good reproducibility and recovery with % RSD less than 2. Thus, the proposed method was found to be rapid, specific, precise, accurate and cost-effective quality control tool for the routine analysis of Sildenafil citrate and Fluoxetine Hydrochloride in bulk and combined dosage form. A rapid and simple derivative spectrophotometric method was developed for simultaneous determination of Sildenafil citrate and Fluoxetine Hydrochloride in tablet dosage form. This method involves second order derivative spectroscopy using 282 nm and 249 nm as zero crossing points for Sildenafil citrate and Fluoxetine Hydrochloride respectively in methanol. Linearity was observed in the concentration range of 10-18µg/ml for Sildenafil citrate and 3-8ug/ml for Fluoxetine Hydrochloride. The accuracy of the method was found to be 98.21% and 99.2% for Sildenafil citrate and Fluoxetine Hydrochloride respectively. The method showed good reproducibility and recovery with % RSD less than 2.Thus, the proposed method was found to be rapid, specific, precise, accurate and cost-effective quality control tool for the routine analysis of sildenafil citrate and Fluoxetine Hydrochloride in bulk and combined dosage form. A selective, precise, isocratic and accurate stability indicating reverse phase high performance liquid chromatographic method was developed for the simultaneous determination of Sildenafil citrate and Fluoxetine Hydrochloride in the tablet dosage form. The method was validated for the linearity, accuracy, precision, robustness, system suitability as per ICH guidelines. Sildenafil citrate and Fluoxetine Hydrochloride were found to be linear in the range of 10-100 and 10-18µg/ml and 3-8ug/ml with the recoveries of 98.6% and 99.2%. The method was also applied for the determination of sildenafil citrate and Fluoxetine Hydrochloride in the presence of their degradation products formed under variety of stress conditions.

Second-Order Derivative Spectrophotometric Method for Simultaneous Estimation of Azilsartan Medoxomil and Cilnidipine in Combined Dosage Form

Second-Order Derivative Spectrophotometric Method for Simultaneous Estimation of Azilsartan Medoxomil and Cilnidipine in Combined Dosage Form

Effective spectrophotometric methods for resolving the superimposed spectra of Diclofenac Potassium and Methocarbamol

The UV spectra of Diclofenac Potassium DIC and Methocarbamol MET are superimposed making their analysis using direct or derivative spectrophotometric methods quite complicated. This study presents four effective spectrophotometric methods that enable simultaneous determination of both drugs without interference. The first method is based on application of simultaneous equation method on their zero order spectra where DIC has shown absorbance maxima at 276 nm and MET displays two absorbances maxima at 273 nm and 222 nm in distilled water. The second method relies on dual wavelength method, the two wavelengths (232 and 285 nm) were chosen for determination of DIC where the absorbance differences at these wavelengths are proportional to DIC concentration while the absorbance differences of MET are equal to zero. For the determination of MET, the two wavelengths (212 and 228 nm) were selected. The third method of first-derivative ratio has been applied where the derivative ratio absorbances of DIC and MET were measured at 286.1 and 282.4 nm, respectively. The fourth method utilizing ratio difference spectrophotometric (RD) method was eventually performed on the binary mixture. The amplitude difference between the two wavelengths (291and 305 nm) was calculated for DIC estimation while the amplitude difference between the two wavelengths (227and 273 nm) for MET determination. All methods show linearity range from 2.0–25 μg. mL−1 and 6.0–40 μg. mL−1 for DIC and MET respectively. The developed methods have been statistically compared with a reported method based on first derivative method and the results of statistical comparison confirm the accuracy and precision of the proposed methods therefore they can be effectively applied for determination of MET and DIC in pharmaceutical dosage form.

Determination of Dextromethorphan Hydreobromide in pharmaceutical preparation using derivative spectrophotometric method

A simple, sensitive, economic, accurate and precise second (D2) and third (D3) derivative spectrophotometric method has been developed for determination of Dextromethorphan hydrobromide in pharmaceutical preparation. The method obeys Beer’s Law in concentration range of 10-50μg/ml employed for evaluation . The quantitative determination of the drug was carried out using the second and third derivative values by measuring ; peak to base line at (300 nm ,240 nm and 228 nm for second derivative) and (303 nm, and 290 nm for third derivative) , peak to peak at ( 300 nm – 240 nm, 240nm – 228nm for second derivative) and (303 nm-290 nm for third derivative) and peak area at (313 nm – 290 nm, 256 nm – 230 nm and 232nm -223nm for second derivative) and at (313 nm -298 nm and 297 nm – 281 nm for third derivative) in 1:10% absolute ethanol: distal water . The results of analysis were validated by recovery studies . The recovery and RSD values was (103.968-97.530 %) and (2.222 – 0.023 %) respectively . The proposed method was applied on syrup formulation (Mini Mond ) .

Smart UV Derivative Spectrophotometric Methods for Simultaneous Determination of Metformin and Remogliflozin: Development, Validation and Application to the Formulation

Abstract: Background: The result of pharmaceutical industry research for the new class and the new combination of drugs for the treatments of diabetes is the newly approved combination of metformin (MET) and remogliflozin (REM). For the quality control of this formulation, three smart, reproducible and non-sophisticated spectroscopic techniques were developed by modification of UV spectra. Materials and Methods: The first two methods were based on the measurements of the peak height of the third derivative and second derivative ratio spectra of MET and REM and the third method was the constant center spectrum subtraction method. Results: The proposed methods exhibited Beer’s law in the range of 2.5 to 30 μg/ml and 1 to 24 μg/ml for MET and REM correspondingly by all three methods. The mean percentage recovery was found to be in the range of 99.08% to 100.15% for MET and 98.73% to 100.27% for REM. Further, both analytes were quantified from the formulation using proposed spectroscopic methods with high accuracy. Comparison of all three methods with the reported HPLC method showed no variation in the assay outcomes in relation to accuracy and precision. Conclusion: The suggested techniques are simple, accurate and reproducible, hence could be used for regular quality control of formulation consisting of MET and REM. Key words: Metformin, Remogliflozin, UV, Derivative spectroscopy, Validation, Formulation.

Derivative Spectrophotometric Method Development and Validation for the Estimation of Evogliptin Tartrate in Pharmaceutical Dosage Form

Abstract: Aim: A simple and economic method was developed as a derivative spectrophotometric study for estimation of evogliptin tartrate in the tablet dosage form. The developed derivative method was validated as per the ICH guideline. Materials and Methods: The maximum absorption of evogliptin tartare was found to be 267 nm and its first and second derivative wavelengths were measured at 275 nm and 277 nm respectively. Water was used as a solvent for all measurements. Results: The developed method was shown linear in the concentration range of 20-120 μg/ml for evogliptin tartrate and shows a good correlation coefficient. The precision of the developed method was less than the maximum allowable limit (% RSD < 2) specified by the ICH guidelines. Excellent % recovery (98% - 101%) with less than 2% RSD value indicates method was accurate. Conclusion: The developed UV – Visible method was simple eco-friendly, precise and accurate as per ICH guidelines. The proposed method will use in quality control for routine analysis of evogliptin tartrate in the pharmaceutical dosage form. Keywords: Derivative method, Evogliptin tartrate (EVO), First derivative, Spectroscopy method, UV-visible method, Validation.

Derivative Spectrophotometric Methods for Determination of Solifenacin Succinate in Bulk and in Tablet Formulation

Derivative Spectrophotometric Methods for Determination of Solifenacin Succinate in Bulk and in Tablet Formulation