scholarly journals Capillary Electrophoresis with UV Detection to Determine Cocaine on Circulated Banknotes

2013 ◽  
Vol 2013 ◽  
pp. 1-7 ◽  
Author(s):  
Melina Heller ◽  
Luciano Vitali ◽  
Mariana A. Siqueira ◽  
Alysson V. F. Sako ◽  
Marcel Piovezan ◽  
...  

A new methodology employing capillary electrophoresis with UV detection (CE-UV) was developed, validated, and applied to determine the presence of cocaine on Brazilian banknotes. Some of the banknotes analyzed were obtained directly from general circulation (well used) while others were collected from Automated Teller Machines (ATMs) (relatively new). The background electrolyte optimized using Peakmaster 5.1 software was composed of 60 mmol L−1 TRIS(hydroxymethyl)aminomethane and 20 mmol L−1 2-hydroxyisobutyric acid, at pH 8.4. The separation time achieved for cocaine was only 2.5 minutes. The figures of merit obtained in the evaluation of the proposed method were good linearity (r>0.999) in the concentration range of 0.8–8.0 mg L−1 and acceptable limits of detection and quantification (0.2 mg L−1 and 0.8 mg L−1, resp.). The relative standard deviations of the instrumental precision, repeatability (intraday), and intermediate precision (interday) were less than 4.5% (peak area). The accuracy evaluated through comparing the cocaine results for the banknotes determined by the proposed CE-UV method and using an LC-MS/MS method showed no significant difference between the methods (95% confidence level). In the analysis of the samples cocaine was detected on 93% of the circulating banknotes in amounts ranging from 11.5 μg to 2761.9 μg per note.

2008 ◽  
Vol 6 (4) ◽  
pp. 617-621 ◽  
Author(s):  
Jinzhang Gao ◽  
Haifeng Fan ◽  
Wu Yang ◽  
Xiangli Sun ◽  
Chongyang Li ◽  
...  

AbstractA rapid, simple and reliable capillary electrophoresis method for the separation and quantitation of inorganic cations with indirect UV detection at 214 nm was developed. The electrolyte was: 12 mM imidazole as background absorbance provider; 5 mM malic acid and 1.0 mM 18-crown-6 ether as complexing agents; and 20% D2O (v/v) to improve ion mobility. The pH was 4.25. The applied voltage was 22 kV at 22°C. Nine ions were completely separated and determined with correlation coefficients of 0.9979-0.9992. The relative standard deviations (RSD) were less than 0.5% for migration time and less than 5.2% for peak area (n=8). The detection limits (S/N=3) were from 0.08 mg L−1 (for Na+) to 0.51 mg L−1 (for Cu2+). To assess the reliability atomic absorption (AA) was also used to determine the same samples. Satisfactory results were obtained for real samples of jasmine tea drink and coconut milk.


2020 ◽  
Vol 58 (9) ◽  
pp. 868-874
Author(s):  
Jie Gong ◽  
Guanglian Zhou ◽  
Yuanhong Wu ◽  
Siying Zhang ◽  
Xiumei Liu

Abstract A capillary electrophoresis (CE) method combined with online and offline enrichment for improving the detection sensitivity of chondroitin sulfate (CS) is established. The online enrichment method is based on the field-amplified sample stacking and large volume electrokinetic injection, and offline enrichment is based on the association between cetyltrimethylammonium chloride and CS. Experimental parameters affecting CE method such as the type and pH of background electrolyte, the injection mode and time and the steps of offline enrichment were optimized. Under optimum conditions, the calibration plot between CS concentration and peak area was linear in the range of 1 ~ 100 μg/mL. The enrichment factor was 130 times and the limit of detection was 50 ng/mL. The average recovery was 103.5% and the relative standard deviation of peak area was <2.0%. The method was successfully applied to the quantitative analysis of CS in drugs.


2006 ◽  
Vol 89 (5) ◽  
pp. 1367-1372 ◽  
Author(s):  
Marinês J Souza ◽  
Rosecler R Kulmann ◽  
LucÊlia M Silva ◽  
Daniele R Nogueira ◽  
Estevan S Zimmermann ◽  
...  

Abstract Cefepime is a new parenteral cephalosporin that has been described as a fourth-generation, broad-spectrum antibiotic. This paper reports the development and in-house validation of an agar diffusion bioassay using a cylinder-plate method for the determination of cefepime in powder for injection. The validation performed yielded good results in terms of linearity, precision, accuracy, and robustness. The assay is based on the inhibitory effect of cefepime upon the strain of Micrococcus luteus ATCC 10240 used as the test microorganism. The results of assays were treated statistically by analysis of variance (ANOVA) and were found to be linear (r = 0.99993) in the selected range of 8.032.0 g/mL; precise [repeatability: relative standard deviation (RSD) = 1.39%, intermediate precision: between-day RSD = 1.77%, and between-analyst RSD = 1.97%] and accurate. Comparison of bioassay and liquid chromatography by ANOVA showed no significant difference between methodologies. The results demonstrated the validity of the proposed bioassay, which is a simple and useful alternative methodology for cefepime determination in routine quality control.


2020 ◽  
pp. 1-7
Author(s):  
Xiaobin Li ◽  
Fangfang Gao ◽  
Huitao Liu ◽  
Yuan Gao

Abstract A simple capillary electrophoresis (CE) method with ultraviolet (UV) detection was developed for the determination of hexachlorophene (HCP) in cosmetics. Separation conditions were obtained in 20 mM Na2B4O7, 10% MeOH (pH 9.20), with 25 kV applied voltage and UV detection at 208 nm. Under the selected conditions, electrophoretic analysis was completed in about 4 min, with limit of detection (LOD) of 0.06 µg·mL−1 for HCP. The method was successfully applied to determine HCP in three kinds of cosmetics with relative standard deviations (RSD) of 0.52–3.02% and recoveries from 90.0 to 96.4% for the spiked samples. The results indicated that the proposed method was reliable. Comparative experiments were also carried out with high-performance liquid chromatography (HPLC)-UV method described in National Standards of People's Republic of China. The validation results of the two methods are comparable, but the proposed CE method is simple, rapid, which makes separation and analyte quantification in shorter time with much less reagent consumption.


Molecules ◽  
2021 ◽  
Vol 26 (22) ◽  
pp. 6931
Author(s):  
Izabella Kośka ◽  
Krystian Purgat ◽  
Rafał Głowacki ◽  
Paweł Kubalczyk

We have developed a precise and accurate method for the determination of ciprofloxacin and ofloxacin in meat tissues. Our method utilizes capillary electrophoresis with a transient pseudo-isotachophoresis mechanism and liquid–liquid extraction during sample preparation. For our experiment, a meat tissue sample was homogenized in pH 7.00 phosphate buffer at a ratio of 1:10 (tissue mass: buffer volume; g/mL). The extraction of each sample was carried out twice for 15 min with 600 µL of a mixture of dichloromethane and acetonitrile at a 2:1 volume ratio. We then conducted the electrophoretic separation at a voltage of 16 kV and a temperature of 25 °C using a background electrolyte of 0.1 mol/L phosphate–borate (pH 8.40). We used the UV detection at 288 nm. The experimentally determined LOQs for ciprofloxacin and ofloxacin were 0.27 ppm (0.8 nmol/g tissue) and 0.11 ppm (0.3 nmol/g tissue), respectively. The calibration curves exhibited linearity over the tested concentration range of 2 to 10 nmol/g tissue for both analytes. The relative standard deviation of the determination did not exceed 15%, and the recovery was in the range of 85–115%. We used the method to analyze various meat tissues for their ciprofloxacin and ofloxacin contents.


2005 ◽  
Vol 88 (4) ◽  
pp. 1059-1063 ◽  
Author(s):  
Ana R Breier ◽  
Sílvia S Garcia ◽  
André Jablonski ◽  
Martin Steppe ◽  
Elfrides E S Schapoval

Abstract A simple, accurate, and effective capillary electrophoresis method with ultraviolet absorbance detection was developed and validated for the quantitation of the antihistamine fexofenadine in capsules. The separation was performed with an uncoated fused-silica capillary (47 cm × 75 μm id) and was operated at 20 kV potential. Temperature was maintained at 25°C. The run buffer was prepared with 20mM Na2B4O7 × 10 H2O. Software was used for system control, data acquisition, and analysis. Method validation was performed by evaluation of the analytical parameters linearity, precision, accuracy, limits of detection and quantitation, and specificity. The method was linear (r = 0.9999) at concentrations ranging from 20 to 100 μg/mL, precise (relative standard deviation intra-assay = 1.2, 1.6, and 1.8% and interassay = 1.5%); accurate (recovery = 98.1%); and specific. The limits of detection and quantitation were 0.69 and 2.09 μg/mL, respectively. The method was compared to the liquid chromatography method developed previously by the authors for the same drug, and no significant difference was found between the 2 methods in fexofenadine hydrochloride quantitation.


2021 ◽  
Vol 63 (11) ◽  
pp. 58-64
Author(s):  
Manh Huy Nguyen ◽  
◽  
Thi Ha Tran ◽  
Minh Tuan Vu ◽  
Thanh Dam Nguyen ◽  
...  

Nowadays, the issue of fresh food, drinks, and residue analysis of toxic compounds in food and drinks is increasingly interested in society. In this study, an analytical procedure for quantitative analysis of the glyphosate residue in beverages such as tea infusion and beer was developed based on the capillary electrophoresis method with capacitively-coupled contactless conductivity detector combined with sample preparation using solid phase extraction technique. The analytical conditions optimised for capillary electrophoresis equipment included: histidine/acetic acid background electrolyte solution with histidine concentration of 1 mM and pH value was adjusted to 2.75 by acetic acid; a separation voltage was 20 kV was applied and a high voltage injection at 20 kV for 10 seconds was chosen. The optimised analytical procedure has resulted in a low detection limit of glyphosate (0.42 μg/l), the repeatability and reproducibility expressed by the relative standard deviation of the peak area and migration time were both less than 10%, a wide linear range, and the obtained recovery efficiency of glyphosate on different drinks were achieved to values ranging from 88.7 to 96.3%.


2020 ◽  
Vol 16 ◽  
Author(s):  
Bathinapatla Ayyappa ◽  
Suvardhan Kanchi ◽  
Myalowenkosi I. Sabela ◽  
Krishna Bisetty

BACKGROUND: Sucralose is a high intensity artificial sweetener sucralose and chemically known as 1,6-dichloro-1,6-dideoxy-β-D-fructofuranosyl-4-chloro-4-deoxy-α-D-galactopyranoside. It is used as a sweetener and flavour enhancer in foods and beverages. Due to its high stability at wider temperatures and pH, made its applicability in various food products throughout the world. As per Joint FAO/WHO Expert Group on Food Additives (JECFA) in 1990, the daily intake of sucralose is 0-15 mg/kg body weight. The literature reports suggest that sucralose has a possible health threat due to the presence of chlorine groups, thereby leading to the several illnesses. The growing interest on the use of SUC in the foods, makes it necessary in developing a fast, reliable, cost effective and reproducible analytical method to determine SUC in food samples. The detection of sucralose and other carbohydrates like fructose, glucose and sucrose is a challenging task owing to its: (i) unavailability of the charged functions and (ii) lack of absorption of strong chromophoric nature in the UV region. Therefore, separation of non-absorbing neutral molecules needs a careful procedure with the suitable electrolyte systems. METHODOLOGY: An indirect UV detection capillary electrophoretic method is described for the separation of sucralose in different food samples. It was achieved by nucleophile substitution (SN2) in the presence of amine as background electrolytes. The morpholine buffer showed good buffering capacity in terms of migration time (< 8.0 min) and baseline stability when compared to other amine buffers (ethylamine, piperidine, triethylamine). The analytical applications of proposed method showed by recovery percentages of sucralose in real and spiked samples on intra and inter-day basis at optimum experimental conditions of 0.2 M buffer concentration and pH 12.0 at 230 nm UV detection. RESULTS: The selection of BGE, UV detection wavelength, buffer concentration, buffer pH, cassette temperature and applied voltage were optimized to enhance the sensitivity and selectivity of the separation method. Recoveries obtained were ranging from 96.87 to 98.82 % for real samples and 94.45 to 98.06 % for spiked samples respectively. Linearity was studied in the range of 2-10 mM, and showed a correlation coefficients of 0.9942 with LOD and LOQ found to be 0.3804 mg L-1 and 1.5215 mg L-1 with % RSD (n = 5) ± 1.27 and 1.19 % with respect to migration time and peak area. Furthermore, to better understand the separation of sucralose with amine buffers were investigated computationally using HOMO-LUMO calculations. The obtained results showed that the band gap decreases in the presence of amine moiety irrespective of its nature. CONCLUSION: In the study, novel background electrolytic system was successfully applied to separate sucralose using indirect UV detector with capillary electrophoresis. The FT-IR results confirmed that the interaction of sucralose with different amine buffers to better understand the separation chemistry behind sucralose and amine complexes. Moreover, computational results indicate that the direction of charge transfer from the amine functionality to the glucofuranosyl ring in each amine derivative of sucralose confirms the strong interaction between sucralose and amines, which led in the baseline separation of sucralose in different food samples.


BMC Chemistry ◽  
2021 ◽  
Vol 15 (1) ◽  
Author(s):  
Ranju Bansal ◽  
Ranjit Singh ◽  
Khushpal Kaur

Abstract Background Environment-friendly fast and accurate mid-infrared spectroscopic methods have been developed for the quantitative analysis of doxorubicin hydrochloride (DOX) and arterolane maleate (ALM) in bulk and marketed formulations. Both transmittance and reflectance modes have been used for the analysis and a comparison has been drawn for better accuracy. The analytical methods were validated in accordance with International Council for Harmonisation (ICH) guidelines Results The proposed methods have been successfully developed and validated for the quantification of doxorubicin and arterolane maleate in solid bulk and dosage form. High recovery values in both the modes, while analysing DOX and ALM, indicated good accuracy of the methods. The methods showed excellent repeatability and intermediate precision [% RSD (Relative Standard Deviation < 2.0%]. The assay values of the drugs in solid dosage forms were also found close to the labelled claim. Conclusion The proposed Fourier transform infrared (FT-IR) spectroscopic methods were found to be specific, reproducible, valid and could be used as general methods for the quantification of most of the solid drug preparations such as tablets, capsules and powders.


2010 ◽  
Vol 25 (5) ◽  
pp. 588-593 ◽  
Author(s):  
Mitsuhiro Kinoshita ◽  
Naotaka Kakoi ◽  
Yu-ki Matsuno ◽  
Takao Hayakawa ◽  
Kazuaki Kakehi

Sign in / Sign up

Export Citation Format

Share Document