scholarly journals Validation of UV Spectrophotometry Method for Determination of Lopinavir and Ritonavir Simultaneously

2021 ◽  
Vol 8 (2) ◽  
pp. 48
Author(s):  
Siti Umi Anisah ◽  
Asri Darmawati ◽  
Amirudin Prawita

Lopinavir and ritonavir are anti-viral compounds that have similar chemical structures and overlapping UV spectral profiles. The combination of these two compounds is being promoted as an anti-COVID19 drug. Determination of these two compounds simultaneously using UV spectrophotometry method requires special technique so that the result will be valid. The purpose of this study was to obtain a suitable analytical technique using UV spectrophotometry for the determination of lopinavir-ritonavir simultaneously that fulfill the method validation requirement. In this study, the simultaneous equation technique, absorptivity comparison factor, and first derivative technique were used to overcome the effect of lopinavir/ritonavir absorbance at selected wavelengths for determination of each compound simultaneously. The one-way ANOVA statistical test was used to compare the result of the three analytical techniques. The results showed that the three techniques fullfilled the AOAC requirements for selectivity and linearity. The accuracy and precision test result have not met the requirements of the AOAC method validation. Statistically. the one-way ANOVA analysis showed there was a significant difference between the mean recovery of lopinavir using the absorptivity factor and first derivative technique. Whereas, there was no significant differences among the mean of ritonavir recoveries that were determined using those three techniques. As conclusion, that the UV spectrophotometric method using the simultaneous equation technique, the absorptivity factor technique, and the derivative technique for assaying the lopinavir and ritonavir simultaneously met the requirements for selectivity and linearity parameters. However, the accuracy and precision have not met the requirements. The first derivative technique is suitable for further developed for ritonavir and lopinavir determination simultaneously

2009 ◽  
Vol 92 (6) ◽  
pp. 1673-1680 ◽  
Author(s):  
marinês J E Souza ◽  
Natália Canedo ◽  
Paulo S Souza Filho ◽  
Ana M Bergold

Abstract A UV spectrophotometric method was developed for determination of ceftiofur sodium in the drug substance and sterile powder for injection. The method validation, which yielded good results, included evaluation of the range, linearity, intraand interday precision, accuracy, recovery, specificity, robustness, LOQ, and LOD. The UV spectrophotometric determinations were performed at 292 nm. Good linearity was obtained between 2.5 and 20.0 g/mL. A prospective validation showed that the method is linear (r = 0.9999) and precise, with RSD values of 0.3 for product A and 0.4 for product B. The intraand interday precision values were <2 for all samples analyzed. Comparison of UV spectrophotometry and LC by analysis of variance and Student's t-test showed no significant difference between methodologies. Moreover, the accuracy and precision obtained with the UV method correlated well with the values obtained with the LC method, and this correlation suggests that UV spectrophotometric analysis can be an inexpensive, reliable, and less time-consuming alternative to chromatographic analysis. The results demonstrated the validity of the proposed method as a simple and useful alternative for the determination of ceftiofur in routine QC analyses.


2020 ◽  
Vol 21 (1) ◽  
pp. 1
Author(s):  
Elisa Almeyda ◽  
Elok Widayanti

Jamu kunir asem merupakan jamu yang bermanfaat untuk meredakan nyeri pada saat menstruasi karena mengandung kurkuminoid yang bersifat analgetika, antipiretika dan antiinflamasi. Tujuan dari penelitian ini yaitu menganalisis perbedaan kadar kurkuminoid pada filtrat, residu dan campuran filtrat-residu jamu kunir asem. Sebanyak 2 gram sampel diekstraksi dengan 40 ml kloroform kemudian diuapkan hingga didapatkan ekstrak dan dilarutkan dengan etanol p.a. Penetapan kadar kurkuminoid pada sampel menggunakan metode Spektrofotometri Uv-Visible pada panjang gelombang 462 nm. Kadar kurkuminoid terendah pada filtrat sebesar 11,346 ppm dan tertinggi pada residu sebesar 49,047 ppm sedangkan campuran filtrat-residu sebesar 22,549 nm. Hasil analisis One Way Anova menunjukkan bahwa  rata-rata konsentrasi kurkuminoid pada campuran filtrat-residu, filtrate dan residu jamu kunir asem berbeda secara signifikan.Kata  kunci: Filtrat; jamu kunir asem; kurkuminoid; residu Analysis of Curcumin Levels in Filtrat, Residuesand Mixed in Herb of Turmeric Tamarind ABSTRACTTurmeric tamarind is a useful herb to relieve pain during menstruation because it contains analgesic, antipyretic and anti-inflammatory curcuminoids. The purpose of this study was to analyze differences in levels of curcuminoids in filtrate, residues and mixture of filtrate residues of tamarind turmeric. A total of 2 grams of sample was extracted with 40 ml of chloroform and then evaporated until an extract was obtained and dissolved with ethanol p.a. Determination of curcuminoid levels in samples using the Uv-Visible Spectrophotometry method at a wavelength of 462 nm. The lowest curcuminoid content in the filtrate was 11.346 ppm and the highest in the residue was 49.047 ppm while the mixture of the filtrate-residue was 22.549 nm. The results of the One Way Anova analysis showed that the mean curcuminoid concentration in the mixture of filtrate-residue, filtrate and residues of tamarind turmeric was significantly different.Keywords: curcuminoids, turmeric tamarind, filtrate, residue


2015 ◽  
Vol 22 (05) ◽  
pp. 648-655
Author(s):  
Bashir Elfatih Abdalla ◽  
Abedelmula M. Abdealla

Objectives: several improvements have been made in the design of immunoassayssuch as method of antibody production, labeling, automation and detection technology. The aim ofthe present study was to compare the accuracy and precision of enzyme linked immunofloriscenceassay (ELFA) and electrochemiluminescence assay (ECL), with Elisa for determination of serum TSHlevels. Period: Feb 2014 to Nov 2014. Setting: College of postgraduate studies, University of Al-Neelain, Khartoum, Sudan. Material and Methods: Three commercial control materials low, normaland high levels of TSH, were used for imprecision studies of immunofloriscence assay (ELFA) andelectrochemiluminescence assay (ECL) methods and 120 patients samples including low (20%),normal (50%), and high (30%) TSH levels, were measured by the two methods, and used for methodscomparison. In addition to six assigned prepared pool serum used for linearity evaluation of the twomethods. Results: Inter- and intra-assay CV% for ECL and ELFA was significantly low compared withthe required by the manufacture. (Intraassay CV% for ECL was 2.9%, 2.74%, and 2.55% for low,normal, and high respectively of TSH levels of the control sera. Intraassay CV% for ELFA was 3.95%,3.75%, and 5.73% for low, normal, and high respectively of TSH levels of the control sera. InterassayCV% for ECL was 3.0%, 2.75%, and 2.81% for low, normal, and high respectively of TSH levels ofthe control sera. Intraassay CV% for ELFA was 4.26%, 4.0% , and 5.75% for low, normal , and highrespectively of TSH levels of the control sera. Although the mean TSH levels of the three levels of thecontrol sera measured by ECL & ELFA methods, is significantly difference from assigned TSH meanvalues( low 0.488+/-0.078,normal 6.016+/- 0.952,high 33.651+/-5.39) , but the measured values iswithin the mean range of the assigned means values. ECL; low (0.611 +/- 0.018. p ≤ 0.001), normal(6.6785 +/- 0.183. p ≤ 0.00), high (35.0485 +/- 0.894. p ≤ 0.02). ELFA low (0.50545 +/- 0.020. p ≤0.00) , normal (6.5395 +/- 0.244. p ≤ 0.00), high (31.0350 +/- 1.779. p ≤0.001).The mean TSH levelsof the 120 patients samples measured by ECL & ELFA , is significantly difference , for ECL (15.74+/-1.181 . p ≤ 0.00) when compared with the mean TSH value (14.56 +/- 1.65) of the patients samples.For ELFA method also there is significant difference (13.76 +/- 1.59 , p ≤ 0.00) when comparedwith mean of the assigned TSH values(14.56 +/- 1.65) of the patients samples, but within the targetvalues of the means .The study showed strong relationship between the two TSH levels measuredby ECL( mean 15.74 mIU/L, slope 0.67 , correlation coefficients 0.991, p ≤ 0.00) and by ELFA (mean 13.76 mIU/L, slope 0.54, correlation coefficients 0.995, p ≤ 0.00) with the assigned values(14.56 ) of 120 patients sample .The results illustrates no significant difference of TSH mean level insix prepared pool samples measured by ECL(22.63 mIU/l +/- 1.12 , p ≤ 0.1) and ELFA(19.87mIU/l+/- 1.15 , p ≤ 0.11) when compared with the TSH assigned values(22.54 mIU/l +/-0.96), and withstrong correlation between the two TSH levels measured by ECL(22.63 mIU/l, slope 0.79, correlationcoefficients 0.999, p ≤ 0.00) and ELFA ( mean 19.87mIU, slope 0.68, correlation coefficients 0.985,p ≤ 0.00), with the assigned TSH values (22.54 mIU/l +/-0.96).of the six prepared pool samples.Conclusion: Considerable significant precision and accuracy was manifested by both ECL and ELFAmethods in estimation of TSH levels, but ECL is more precise than ELFA especially in the lower TSHconcentration.


2018 ◽  
Vol 9 ◽  
pp. 67
Author(s):  
Gina Maringka ◽  
Bambang Irawan ◽  
Ellyza Herda ◽  
Zainal Alim Masud

Objective: The aim of this study was to prove that organic solvents areas effective and efficient as sandblasting and burning for cleaning rebonded brackets.Methods: Thirty stainless steel metal brackets mounted on 30 maxillary first premolar teeth were categorized into three cleaning method groups, each consisting of 10 brackets. After 24 h, shear bond strength (SBS) tests were performed using a universal testing machine.Results: The one-way ANOVA test showed a significant difference (p=0.000) among the mean SBS values in the three cleaning method groups. However, the modified adhesive remnant index by a Kruskal–Wallis analysis showed no significant difference (p=0.860). The scanning electron microscopy results revealed that the organic solvent cleaning method showed better bracket performance than the other two methods. Moreover, the energy-dispersive X-ray spectroscopy results showed that the adhesive material remaining on the bracket base was relatively similar among the three cleaning methods.Conclusion: Based on practicality and the results of this study, the organic solvent cleaning method was proven to be effective and efficient. Therefore, organic solvents can be recommended as an alternative cleaning method for detached brackets.


2015 ◽  
Vol 98 (1) ◽  
pp. 35-45 ◽  
Author(s):  
Nadia M Mostafa ◽  
Laila Abdel-Fattah ◽  
Soheir A Weshahy ◽  
Nagiba Y Hassan ◽  
Shereen A Boltia

Abstract Five simple, accurate, precise, and economical spectrophotometric methods have been developed for thedetermination of cefixime trihydrate (CFX) in the presence of its acid and alkali degradation products without prior separation. In the first method, secondderivative (2D) and first derivative (1D) spectrophotometry was applied to the absorption spectra of CFX and its acid (2D) or alkali (1D) degradation products by measuring the amplitude at 289 and 308 nm, respectively. The second method was a first derivative (1DD) ratio spectrophotometric method where the peak amplitudes were measured at 311 nm in presence of the acid degradation product, and 273 and 306 nm in presence of its alkali degradation product. The third method was ratio subtraction spectrophotometry where the drug is determined at 286 nm in laboratory-prepared mixtures of CFX and its acid or alkali degradation product. The fourth method was based on dualwavelength analysis; two wavelengths were selected at which the absorbances of one component were the same, so wavelengths 209 and 252 nm were used to determine CFX in presence of its acid degradation productand 310 and 321 nm in presence of its alkali degradation product. The fifth method was bivariate spectrophotometric calibration based on four linear regression equations obtained at the wavelengths 231 and 290 nm, and 231 and 285 nm for the binary mixture of CFX with either its acid or alkali degradation product, respectively. The developed methods were successfully applied to the analysis of CFX in laboratory-prepared mixtures and pharmaceutical formulations with good recoveries, and their validation was carried out following the International Conference on Harmonization guidelines. The results obtained were statistically compared with each other and showed no significant difference with respect to accuracy and precision.


1996 ◽  
Vol 75 (05) ◽  
pp. 772-777 ◽  
Author(s):  
Sybille Albrecht ◽  
Matthias Kotzsch ◽  
Gabriele Siegert ◽  
Thomas Luther ◽  
Heinz Großmann ◽  
...  

SummaryThe plasma tissue factor (TF) concentration was correlated to factor VII concentration (FVIIag) and factor VII activity (FVIIc) in 498 healthy volunteers ranging in age from 17 to 64 years. Immunoassays using monoclonal antibodies (mAbs) were developed for the determination of TF and FVIIag in plasma. The mAbs and the test systems were characterized. The mean value of the TF concentration was 172 ± 135 pg/ml. TF showed no age- and gender-related differences. For the total population, FVIIc, determined by a clotting test, was 110 ± 15% and the factor VIlag was 0.77 ± 0.19 μg/ml. FVII activity was significantly increased with age, whereas the concentration demonstrated no correlation to age in this population. FVII concentration is highly correlated with the activity as measured by clotting assay using rabbit thromboplastin. The ratio between FVIIc and FVIIag was not age-dependent, but demonstrated a significant difference between men and women. Between TF and FVII we could not detect a correlation.


2006 ◽  
Vol 3 (3) ◽  
pp. 142-145
Author(s):  
P. Ravi Kumar ◽  
P. Bhanu Prakash ◽  
M. Murali Krishna ◽  
M. Santha Yadav ◽  
C. Asha Deepthi

Domperidone is an antiemetic and pantoprazole is an antiulcer drug. Simple, precise, rapid and selective simultaneous equation and Q- analysis UV spectrophotometric methods have been developed for the simultaneous determination of domperidone and pantoprazole from combined tablet dosage forms. The methods involve solving of simultaneous equations and Q-value analysis based on measurement absorptivity at 216, 287 and 290 nm respectively. Linearity lies between 1-15 mcg/mL for domperidone and 0-50 mcg/mL for pantoprazole.


Author(s):  
Nesma M Fahmy ◽  
Adel M Michael

Abstract Background Modern built-in spectrophotometer software supporting mathematical processes provided a solution for increasing selectivity for multicomponent mixtures. Objective Simultaneous spectrophotometric determination of the three naturally occurring antioxidants—rutin(RUT), hesperidin(HES), and ascorbic acid(ASC)—in bulk forms and combined pharmaceutical formulation. Method This was achieved by factorized zero order method (FZM), factorized derivative method (FD1M), and factorized derivative ratio method (FDRM), coupled with spectrum subtraction(SS). Results Mathematical filtration techniques allowed each component to be obtained separately in either its zero, first, or derivative ratio form, allowing the resolution of spectra typical to the pure components present in Vitamin C Forte® tablets. The proposed methods were applied over a concentration range of 2–50, 2–30, and 10–100 µg/mL for RUT, HES, and ASC, respectively. Conclusions Recent methods for the analysis of binary mixtures, FZM and FD1M, were successfully applied for the analysis of ternary mixtures and compared to the novel FDRM. All were revealed to be specific and sensitive with successful application on pharmaceutical formulations. Validation parameters were evaluated in accordance with the International Conference on Harmonization guidelines. Statistical results were satisfactory, revealing no significant difference regarding accuracy and precision. Highlights Factorized methods enabled the resolution of spectra identical to those of pure drugs present in mixtures. Overlapped spectra of ternary mixtures could be resolved by spectrum subtraction coupled FDRM (SS-FDRM) or by successive application of FZM and FD1M.


2019 ◽  
Vol 2019 ◽  
pp. 1-11
Author(s):  
Shilan A. Omer ◽  
Nabil A. Fakhre

In this study, three simple and accurate spectrophotometric methods for simultaneous determination of pyriproxyfen and chlorothalonil residues in cucumbers and cabbages grown in experimental greenhouse were studied. The first method was based on the zero-crossing technique measurement for first and second derivative spectrophotometry. The second method was based on the first derivative of the ratio spectra. However, the third method was based on mean centering of ratio spectra. These procedures lack any previous separation steps. The calibration curves for three spectrophotometric methods are linear in the concentration range of 1–30 μg·mL−1 and 0.5–7 μg·mL−1 for pyriproxyfen and chlorothalonil successively. The recoveries ranged from 82.12–97.40% for pyriproxyfen and 81.51–97.04% for chlorothalonil with relative standard deviations less than 4.95% and 5.45% in all instances for pyriproxyfen and chlorothalonil, respectively. The results obtained from the proposed methods were compared statistically by using one-way ANOVA, and the results revealed there were no significant differences between ratio spectra and mean centering methods with the zero-crossing technique. The proposed methods are successfully applied for the simultaneous estimation of the residue of both pesticides in cucumber and cabbage samples.


2012 ◽  
Vol 18 (2) ◽  
pp. 339-347 ◽  
Author(s):  
Sameer Abdulrahman ◽  
Kanakapura Basavaiah

Two simple, sensitive and extraction-free spectrophotometric methods are described for the determination of dothiepin hydrochloride (DOTH) both in pure form and in pharmaceutical tablets. The methods are based on ion-pair complex formation between dothiepin base (DOT) and two acidic dyes, namely, bromophenol blue (BPB) or bromocresol green (BCG) with absorption maximum at 425 nm for BPB method or 430 nm for BCG method. Beer?s law is obeyed over the concentration ranges of 1.0-15.0 and 1.0-17.5 ?g mL-1 DOT for BPB and BCG methods, respectively. The molar absorptivity values and Sandell?s sensitivity values are reported for both methods. The limits of detection (LOD) and quantification (LOQ) were calculated to be 0.18 and 0.53 ?g mL-1 for BPB method, and 0.17 and 0.50 ?g mL-1 for BCG method, respectively. The stoichiometry of the complex in either case was found to be 1: 1 and the conditional stability constant (KF) of the complexes has also been calculated. The proposed methods were applied successfully to the determination of DOTH in pure form and in its tablet form with good accuracy and precision. Statistical comparison of the results was performed using Student's t-test and variance ratio F-test at 95% confidence level and there was no significant difference between the official and proposed methods with regard to accuracy and precision. Further, the validity of the proposed methods was confirmed by recovery studies via standard addition technique.


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