scholarly journals Simultaneous Determination and Stability Studies on Diminazene Diaceturate and Phenazone Using Developed Derivative Spectrophotometric Method

2017 ◽  
Vol 2017 ◽  
pp. 1-6 ◽  
Author(s):  
Ruaa Mohamed Akode ◽  
Shaza Wagiealla Shantier ◽  
Elrasheed Ahmed Gadkariem ◽  
Magdi Awadalla Mohamed

This work presents UV first derivative spectrophotometry as a precise, accurate, and feasible method for simultaneous determination of diminazene diaceturate and phenazone in bulk and dosage forms. The absorbance values of diminazene diaceturate and phenazone aqueous mixture were obtained at 398 nm and 273 nm, respectively. The developed method was proved to be linear over the concentration ranges (2–10) μg/mL and (2.496–12.48) μg/mL for diminazene diaceturate and phenazone, respectively, with good correlation coefficients (not less than 0.997). The detection and quantitation limits were found to be (LOD = 0.63 and 0.48 μg/mL; LOQ = 1.92 and 1.47 μg/mL, resp.). The developed method was employed for stability studies of both drugs under different stress conditions. Diminazene diaceturate was prone to degrade at acidic pH via first-order kinetics. The degradation process was found to be temperature dependent with an activation energy of 7.48 kcal/mole. Photo-stability was also investigated for this drug.

1995 ◽  
Vol 41 (3) ◽  
pp. 361-366 ◽  
Author(s):  
A Andersson ◽  
A Lindgren ◽  
B Hultberg

Abstract Changes in concentration of reduced and oxidized low-M(r) thiols were measured in blood and plasma before and after the separation of blood cells. If centrifugation of blood was postponed, the reduced form of homocysteine in plasma increased with time at 22 degrees C; in contrast, the concentrations of other reduced thiols (cysteine, glutathione, and cysteinylglycine) decreased. In plasma the reduced forms of all thiols disappeared at a rate that followed first-order kinetics. The rates of disappearance ("half-lives") were temperature-dependent; they were about the same for glutathione and homocysteine (11.7 and 14.3 min, respectively, at 22 degrees C) and somewhat higher for cysteinylglycine and cysteine. After establishing proper sampling conditions for reduced thiols, we measured this thiol fraction as well as free (non-protein-bound) and total thiols in 10 reference subjects and 19 patients with cerebral infarction. Mild but significant hyperhomocysteinemia involving total and free homocysteine (but not reduced homocysteine) was found in the patients.


Author(s):  
V Phani Kumar ◽  
Y Sunandamma

A high performance liquid chromatographic method with UV detection was developed and validated for simultaneous determination of Pioglitazone and Clopidogrel. Separation was performed on a C18 column by isocratic elution with a mobile phase of Methanol: Acetonitrile: Water (80:10:10) at pH 4.6. The UV detection was set at 230 nm. The method proved to be specific, accurate, precise and linear over the concentration ranges of 20-120ppm for both Pioglitazone and Clopidogrel with correlation coefficients always >0.999 for both drugs. The intra-day and inter-day precision and accuracy were less than 2 for both analytes. DOI: http://dx.doi.org/10.3329/ijpls.v2i1.14580 International Journal of Pharmaceutical and Life Sciences Vol.2(1) 2013: 1-9


2016 ◽  
Vol 99 (4) ◽  
pp. 923-928 ◽  
Author(s):  
Ali Kemal Fidan ◽  
Sezgin Bakirdere

Abstract A sensitive analytical method was developed for the simultaneous determination of sildenafil and tadalafil in legal drugs, illicit/counterfeit drugs, and wastewater samples. Chromatographic separation of two analytes was achieved on a C18 column with a mobile phase including 50 mM phosphate buffer at pH 6.0 and acetonitrile (35 + 65, v/v) at the flow rate of 1.0 mL/min. Analytes were separated from each other in 6 min with high resolution. LOD/LOQ values were calculated as 28/92 ng/mL for sildenafil citrate and 39/129 ng/mL for tadalafil. Calibration plots for both analytes were linear with correlation coefficients >0.9993. A validated method was successfully applied to legal and illicit erectile-dysfunction drug samples consumed in Istanbul, Turkey, and to wastewater samples. Nine different samples were analyzed for qualitative and quantitative measurement of their ingredients, and the results were compared with the values written on the labels of the drugs. The wastewater sample was also analyzed for its sildenafil and tadalafil content. To calculate the recoveries, a spiking experiment was performed and recovery rates for sildenafil and tadalafil were calculated as 101.30 ± 3.43 and 102.68 ± 1.59, respectively.


2020 ◽  
Vol 32 (2) ◽  
pp. 145-148 ◽  
Author(s):  
Siyuan Chen ◽  
Jianshe Ma ◽  
Xianqin Wang ◽  
Peiwu Geng

Hair is a stable specimen and has a longer detection window (from weeks to months) than blood and urine. Through the analysis of hair, the long-term information of the drug use of the identified person could be explored. Our work is to establish an ultra-performance liquid chromatography–tandem mass spectroscopy (UPLC–MS/MS) method for simultaneous determination of methamphetamine, amphetamine, morphine, monoacetylmorphine, ketamine, norketamine, 3,4-methylenedioxymethamphetamine (MDMA), and 3,4-methylenedioxyamphetamine (MDA) in hair. Methoxyphenamine was used as an internal standard. The chromatographic separation was performed on a UPLC ethylene bridged hybrid (BEH) C18 (2.1 mm × 50 mm, 1.7 μm) column using a mobile phase of acetonitrile–water with 10 mmol/L ammonium acetate solution which containing 0.05% ammonium hydroxide. The multiple reaction monitoring in positive electrospray ionization was used for quantitative determination. The intra-day and inter-day precisions (relative standard deviation [RSD]) were below 15%. The accuracy ranged between 85.5% and 110.4%, the average recovery rate was above 72.9%, and the matrix effect ranged between 92.7% and 109.2%. Standard curves were in the range of 0.05–5.0 ng/mg, and the correlation coefficients were greater than 0.995. The established UPLC–MS/MS method was applied to analyze the hair samples successfully.


2012 ◽  
Vol 554-556 ◽  
pp. 2037-2040
Author(s):  
Yu Qin Li ◽  
Jing Zhao ◽  
Rui Duan ◽  
Bao Xiu Jia ◽  
Gui Rong You ◽  
...  

A reversed-phase high performance liquid chromatographic method was established for the simultaneous determination of tanshinones in three processing products of white flower Radix salvia miltiorrhiza. Cryptotanshinone, tanshinone IA and tanshinone IIA were successfully separated on a Yilite C18 column (250 mm x 4.6 mm, 5 µm). The mobile phase was a mixture of methanol, water, tetrahydrofuran and glacial acetic acid (70:24:5:1, v/v/v/v), employing isocratic elution at a flow rate of 1.0 mL/min. Detection was 254 nm. Regression equations revealed good linear relationship between the peak areas of the compounds and their concentrations (correlation coefficients: 0.9994 for cryptotanshinone, 0.9996 for tanshinone I A and 0.9996 for tanshinone IIA). The recoveries were between 98.03 % and 103.1 %. The method is simple, accurate and effective and can be used to determine the contents of tanshinones in processing products of Salvia miltiorrhiza bge. f. alba, and the contents of three tanshinones presented the stir-frying processing<the crude drugs<the wine prosessing.


1997 ◽  
Vol 126 (1-2) ◽  
pp. 153-157 ◽  
Author(s):  
Luis Fermín Capitán-Vallvey ◽  
Natalia Navas Iglesias ◽  
Ignacio de Orbe Payá ◽  
Ramiro Avidad Castaneda

2018 ◽  
Vol 3 (2) ◽  
pp. 62
Author(s):  
Ariya Wijaya Putra ◽  
Asri Darmawati ◽  
Juniar Mochtar

Background: Sodium benzoate and sodium cyclamate are foods additives generally used as preservative and artificial sweeteners, respectively. Monitoring of sodium benzoate and sodium cyclamate need appropriate analytical method. Objective: The main objective of this study was to gain the optimum conditions for simultaneous determination of sodium benzoate and sodium cyclamate in soft drink by High Performance Liquid Chromatography. Methods: Measurement of the additives was performed in µ-Bondapak RP18 column using methanol:phosphate buffer of pH 4 (42:58) as mobile phase with flow rate of 1 mL/minute. Results: It has shown that correlation coefficients (r) of sodium benzoate and sodium cyclamate was 0.9997 and 0.9991 respectively. Recoveries of the two analyst were acceptable. Conclusions: Five out of nine samples tested contained sodium cyclamate higher than the recommended concentration. All sodium benzoate containing samples were within the recommended concentration.


2020 ◽  
Vol 103 (1) ◽  
pp. 117-123
Author(s):  
Qingling Xie ◽  
Bin Li ◽  
Feibing Huang ◽  
Mengru Cao ◽  
Hanwen Yuan ◽  
...  

Abstract Background: Bupi Yiqi No. 1 Recipe (BPYQ), a traditional Chinese medicine formula, has been widely used as a treatment of multidrug resistance during chemotherapy in colorectal cancer and for the prevention of gastrointestinal cancer recurrence for decades. Objective: In this study, a rapid, reliable, and accurate ultrahigh-performance LC (UHPLC) coupled with electrospray ionization (ESI)–tandem MS (MS/MS) method was developed for the simultaneous determination of 12 major bioactive components, including protocatechuic acid, astilbin, rutin, calycosin-7-O-β-D-glucoside, ginsenoside Re, ononin, isoliquiritigenin, calycosin, apigenin, ginsenoside Rb1, formononetin, and glycyrrhizic acid in BPYQ. Methods: The chromatographic separation of the analytes was achieved on a Poroshell 120 SB-Aq column (50 × 2.1 mm, 1.7 µm) with a mobile phase of acetonitrile and 0.1% (v/v) formic acid aqueous solution. The flow rate and column temperature were set at 0.4 mL/min and 30°C, respectively. Mass spectrometric detection of the analyses was performed on multiple reaction monitoring mode in positive and negative ESI mode. Results: The established UHPLC–ESI–MS/MS method was validated in terms of the linearity, precision, repeatability, stability, and accuracy. All calibration curves of the 12 compounds showed good linearity, with correlation coefficients (r) greater than 0.9980 within the test ranges. The LODs and LOQs for the 12 compounds were in the ranges of 0.08–1.32 and 0.27–5.28 ng/mL, respectively. The average recoveries of all the standard compounds were between 98.4 and 102.9%, and their relative SD values ranged from 1.24 to 3.78%. Conclusions: The proposed method can provide a meaningful basis for the QC of BPYQ. Highlights: The established UHPLC-ESI-MS/MS method was demonstrated to be a powerful tool for quantifying the 12 compounds in BPYQ.


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