A Method for the Determination of Atropine in Pharmaceutical Preparation Using CE-ECL

2014 ◽  
Vol 989-994 ◽  
pp. 1007-1010 ◽  
Author(s):  
Qian Xiang ◽  
Xiao Dong Yang ◽  
Ying Gao
Keyword(s):  
Pharmaceutical Preparation ◽  
Pharmaceutical Preparations ◽  
Peak Height ◽  
Regression Coefficients ◽  
Determination Method ◽  
Analyte Concentration ◽  
Calibration Equation ◽  
Standard Curve ◽  
Sensitive Determination

In this paper, a sensitive determination method for atropine based on end-column electrochemiluminescence of tris (2,2’-bipyridyl) ruthenium (II) detection is described. The conditions affecting separation and detection were investigated. Favorable ECL intensity of atropine was achieved in a solution consisting 5 mmol/L Ru (bpy)32+ and 50 mmol/L phosphate at applied voltage of 1.20V. The standard curve was linear between 1 and 20 μmol/L for atropine. The calibration equation and regression coefficients were: y = 128.38x−36.76 and R = 0.998 in terms of peak height response as a function of analyte concentration. A detection limit of 5×10−8 mol/L (S/N= 3) was achieved. The proposed method was applied satisfactorily to the determination of atropine in three pharmaceutical preparations.

scholarly journals Stability indicating HPLC-Fluorescence detection method for the simultaneous determination of linagliptin and empagliflozin in their combined pharmaceutical preparation

2021 ◽  
Vol 12 (2) ◽  
pp. 168-178
Author(s):  
Mohamed Rizk ◽  
Ali Kamal Attia ◽  
Heba Yosry Mohamed ◽  
Mona Elshahed
Keyword(s):  
Fluorescence Detection ◽  
Mobile Phase ◽  
Pharmaceutical Preparation ◽  
Pharmaceutical Preparations ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Significant Difference

A sensitive, accurate, and precise liquid chromatographic method has been developed and validated for the determination of Linagliptin (LNG) and Empagliflozin (EMP) in their combined tablets. Chromatographic separation was carried out on ODS-3 Inertsil® C18 column (150×4.6 mm, 5 µm). The mobile phase A (consisting of 0.30% Triethyl amine buffer (TEA) at pH = 4.5, adjusted using ortho-phosphoric acid); the mobile phase B (consisting of acetonitrile) was pumped through the column whose temperature was maintained at 40 °C, with a flow rate 1.7 mL/min, using gradient elution from 0-3 min A:B (75:25, v:v), then from 3-6 min the ratio changed to be A:B (60:40, v:v). Fluorescence detection (FLD) was performed at 410 nm after excitation at 239 nm. Acceptable linearity, accuracy and precision values of the proposed method were found over the concentration ranges of 0.5-15 µg/mL for LNG and 1.0-30 µg/mL for EMP with correlation coefficients of 0.9997 and 0.9998 in the case of LNG and EMP, respectively. The recoveries and relative standard deviations percentages were found in the following ranges: 98.56-101.85 and 0.53-1.52% for LNG and 98.00-101.95 and 0.31-1.05% for EMP. The detection and quantification limits were 0.15 and 0.45 µg/mL for LNG and 0.22 and 0.67 µg/mL for EMP. The optimized method was validated and proved to be specific, robust, accurate and reliable for the determination of the drugs in pure form or in their combined pharmaceutical preparations. No significant difference was found regarding accuracy and precision upon statistical comparison between the obtained results of the proposed method and those of the reported method. Furthermore, the proposed method is proved to be a stability-indicating assay after exposure of the studied drugs to variable forced degradation parameters, such as acidic, alkaline and oxidative conditions, according to the recommendations of the International Conference on Harmonization guidelines. The simplicity and selectivity of the proposed method allows its use in quality control laboratories.

scholarly journals Synthesis and Application of a New Thiazolylazo Reagent for Cloud Point Extraction and Determination of Cobalt in Pharmaceutical Preparations

2011 ◽  
Vol 94 (4) ◽  
pp. 1304-1309 ◽  
Author(s):  
Regina Terumi Yamaki ◽  
Luana Sena Nunes ◽  
Hygor Rodrigues De Oliveira ◽  
André S Araújo ◽  
Marcos Almeida Bezerra ◽  
...  
Keyword(s):  
Cloud Point ◽  
Inductively Coupled Plasma ◽  
Cloud Point Extraction ◽  
Pharmaceutical Preparation ◽  
Pharmaceutical Preparations ◽  
Absorption Spectrometry ◽  
Emission Spectrometry ◽  
Preconcentration Procedure ◽  
Flame Atomic Absorption

Abstract The synthesis and characterization of the reagent 2-(5-bromothiazolylazo)-4-chlorophenol and its application in the development of a preconcentration procedure for cobalt determination using flame atomic absorption spectrometry after cloud point extraction is presented. This procedure is based on cobalt complexing and entrapment of the metal chelates into micelles of a surfactant-rich phase of Triton X-114. The preconcentration procedure was optimized by using a response surface methodology through the application of the Box-Behnken matrix. Under optimum conditions, the procedure determined the presence of cobalt with an LOD of 2.8 μg/L and LOQ of 9.3 μg/L. The enrichment factor obtained was 25. The precision was evaluated as the RSD, which was 5.5% for 10 μg/L cobalt and 6.9% for 30 μg/L. The accuracy of the procedure was assessed by comparing the results with those found using inductively coupled plasma-optical emission spectrometry. After validation, the procedure was applied to the determination of cobalt in pharmaceutical preparation samples containing cobalamin (vitamin B12).

Rapid Fluorometric Determination of Benzo(a)pyrene in Foods

1982 ◽  
Vol 45 (2) ◽  
pp. 139-142 ◽  
Author(s):  
YASUHIDE TONOGAI ◽  
SHUNJIRO OGAWA ◽  
MASATAKE TOYODA ◽  
YOSHIO ITO ◽  
MASAHIRO IWAIDA
Keyword(s):  
Detection Limit ◽  
Peak Height ◽  
Excitation Wavelength ◽  
Activated Alumina ◽  
Fluorometric Method ◽  
Fluorometric Determination ◽  
Standard Curve ◽  
Layer Chromatography ◽  
Entire Procedure

A simple and rapid fluorometric method for determining benzo (a) pyrene in foods was developed. Benzo (a) pyrene is extracted from foods with n-hexane:ether mixture (4:1), purified through a column of activated alumina and determined fluorometrically. An excitation wavelength of 295 nm and emission wavelength of 403 nm were used for calculating concentrations of benzo (a) pyrene. The peak height at 403 nm and baseline between 392 and 418 nm were employed to derive a standard curve for quantitating benzo (a) pyrene. A calibration curve for between 0.04 – 4 ng/ml of benzo (a) pyrene was used. Recoveries of benzo (a) pyrene from 14 kinds of food spiked at levels of 20 and 2ppb were within the range of 79.5 – 93.8% and 50.0 – 80.6%, respectively. The entire procedure takes only one hour with the detection limit being 0.1 ppb. Benzo (a) pyrene detected was reconfirmed by thin-layer chromatography.

scholarly journals Automatic continuous on-line monitoring of salicylic acid and acetylsalicylic acid in pharmaceuticals

1990 ◽  
Vol 12 (6) ◽  
pp. 263-266 ◽  
Author(s):  
J. M. López Fernández ◽  
M. D. Luque de Castro ◽  
M. Valcárcel
Keyword(s):  
Salicylic Acid ◽  
Acetylsalicylic Acid ◽  
Simultaneous Determination ◽  
Pharmaceutical Preparation ◽  
Pharmaceutical Preparations ◽  
Sampling Frequency ◽  
The Other ◽  
Dissolution Test ◽  
On Line

An asymmetrical FIA merging-zones manifold based on the dual injection of two sample microvolumes was developed for the simultaneous determination of salicylic acid and acetylsalicylic acid in pharmaceutical preparations at a sampling frequency of 30/h. The complex formed between the Fe(III) reagent continuously introduced in the system and salicylic acid was monitored photometrically at 520 nm. One of the sample plugs was prehydrolysed on injection into an NaOH stream and was circulated through a longer channel than the other plug. This yielded two FIA peaks corresponding to salicylic acid and the overall content, respectively. The proposed manifold was successfully used to control the dissolution test of a pharmaceutical preparation.

A New, Rapid And Sensitive Determination Of Fibrinopeptide- A (FPA) By A High Affinity Antibody To FPA Antiserum

1981 ◽  
Author(s):  
G Stehle ◽  
J Harenberg ◽  
H Schmidtgayk ◽  
R Zimmermann
Keyword(s):  
Rabbit Serum ◽  
Normal Rabbit Serum ◽  
Standard Curve ◽  
High Affinity ◽  
Microtiter Plates ◽  
Highly Sensitive ◽  
Ethanolic Extraction ◽  
Sensitive Determination ◽  
Radioimmunological Determination

The clinical relevance of the determination of FPA is not yet fully recognized because of the still time consuming radioimmunological techniques. Shortening of the incubation times allways lead to a critical loss of the sensitivity of the assay. We present now a modification which provides highly sensitive and reproducable results within 2hrs.The ethanolic extraction of FPA from plasma was shortened to 20 min including centrifugation. Samples were analysed in triplicates and evaporated at 50°C on microtiter plates. The addition of 0.2μl normal rabbit serum (NRS) lead to a 20% increase of the reaction rate of the FPA antiserum to FPA. A second antibody with high affinity to rabbit immunglobulin i.e. the FPA antiserum improved the maximal binding to 35% after an incubation period of only 10 min. 35-40000 cpm tracer FPA were added to each sample. FPA antiserum, second antibody and NRS were preincubated for 1-24 hrs and then added together with the tracer to the samples. Thus a sensitive standard curve was obtained between 0.16 and 160 ng/ml (12000-600 cpm). The correlation coefficient of this modification to our previously described method was r=0.96 (n=60) The variation coefficient could be improved substantially to 3.1 for low, 4.0 for medium and 4.5% for high FPA. Normal FPA were measured between 0.16 and 2.5 ng/ml (mean 1.4 ng/ml, n=32).The presented modification of the radioimmunological determination of FPA overcomes the difficulties of previously described methods and provides acurate results within 2 hrs.

Determination of amino acids in jams, fruits and pharmaceutical preparations by gas chromatography using trifluoroacetylacetone and ethylchloroformate as derivatizing reagents

2015 ◽  
Vol 7 (7) ◽  
pp. 3148-3156 ◽  
Author(s):  
S. A. Majidano ◽  
M. Y. Khuhawar ◽  
R. A. Zounr ◽  
A. H. Channar ◽  
T. M. Jahangir ◽  
...  
Keyword(s):  
Amino Acids ◽  
Gas Chromatography ◽  
Pharmaceutical Preparation ◽  
Pharmaceutical Preparations ◽  
Flame Ionization Detection ◽  
Ionization Detection ◽  
Flame Ionization

A gas chromatography (GC)-flame ionization detection procedure was used to determine amino acids in a pharmaceutical preparation (Aminess N tablets), jams, juices and a vegetable.

Chemiluminescence Enhancement Effect for the Determination of Acetaminophen with the Catalysis of Manganese Deuteroporphyrin (Mn(III)DP)

2013 ◽  
Vol 575-576 ◽  
pp. 249-252 ◽  
Author(s):  
Ying Jun Chao ◽  
Liang Xiao Xie ◽  
Wei Cao
Keyword(s):  
Detection Limit ◽  
Pharmaceutical Preparations ◽  
Peak Height ◽  
Enhancement Effect ◽  
Optimum Conditions ◽  
Chemiluminescence Intensity ◽  
Relative Standard ◽  
Alkaline Conditions ◽  
Flow Injection Chemiluminescence

It is found thatManganese Deuteroporphyrin (Mn(Ⅲ)DP) can greatly enhance the chemiluminescence intensity of luminol-hydrogen peroxide system in alkaline conditions. Basing on that fact a flow injection chemiluminescence (CL) method has been developed for the determination of acetaminophen. With the peak height as a quantitative parameter applying optimum conditions, the relative CL intensity was linear with acetaminophen concentration in the range of 1.0×10-9～1.0×10-7 g/mL with a detection limit of 2.8×10-10 g/mL. The relative standard deviation (RSD) was 2.7% for 2.0 x10-8 g/mL acetaminophen (n = 11). The proposed method held low detection limit and was successfully applied to determination of acetaminophen in pharmaceutical preparations.

Optimisation and validation of liquid chromatographic and partial least-squares-1 methods for simultaneous determination of enalapril maleate and nitrendipine in pharmaceutical preparations

2011 ◽  
Vol 65 (6) ◽  
Author(s):  
Mehmet Caglayan ◽  
Ismail Palabiyik ◽  
Mustafa Bor ◽  
Feyyaz Onur
Keyword(s):  
Least Squares ◽  
Simultaneous Determination ◽  
Partial Least Squares ◽  
Pharmaceutical Preparation ◽  
Pharmaceutical Preparations ◽  
Data Matrix ◽  
Concentration Data ◽  
Enalapril Maleate ◽  
Nm Range

AbstractSimultaneous determination of enalapril maleate (ENA) and nitrendipine (NIT) in pharmaceutical preparations was performed using liquid chromatography (LC) and the partial least-squares-1 (PLS-1) method. In LC, the separation was achieved on a C8 column and the optimum mobile phase for good separation in a gradient elution programme was found to be acetonitrile-water (φ r = 81: 19) and optimum flow-rate, temperature, injection volume, and detection wavelength were set at 1.0 mL min−1, 25°C, 10 μL, and 210 nm, respectively. Dienogest was selected as an internal standard. In the spectrophotometry, a PLS-1 chemometric method was used. The absorbance data matrix related to the concentration data matrix was established by measurement of absorbances in their zero order spectra with an increment of Δλ = 1 nm in the 220–290 nm range for ENA and with Δλ = 1 nm in the 230–290 nm range for NIT in the PLS-1 method. Following this step, calibration was established by using this data matrix to predict the unknown concentrations of ENA and NIT in their binary mixture. These optimised methods were validated and successfully applied to a pharmaceutical preparation in tablet form and the results were subjected to comparison.

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