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1.
Talanta ; 217: 120987, 2020 Sep 01.
Article in English | MEDLINE | ID: mdl-32498887

ABSTRACT

Cocaine is one of the most frequently used illicit drug in the world. Therefore, the development of simple and fast methods for the detection of cocaine and common adulterants, diluents and impurities are extremely important in forensic investigations. The present study describes, for the first time, a method based on capillary electrophoresis with capacitively coupled contactless conductivity detection (CE-C4D) for the rapid (2.5 min) and simultaneous quantification of cocaine, levamisole, lidocaine, carbonate, borate, chloride, nitrate, nitrite and sulphate. In the experiment, anions were separated in co-electroosmotic mode and cations in counter-electroosmotic mode employing a buffer solution composed by 10.0 mmol L-1 TAPS, 12 mmol L-1 NaOH and 0.2 mmol L-1 CTAB as the background electrolyte (pH = 8.8). The developed CE method demonstrated some interesting analytical characteristics such as: (i) a simple sample pretreatment step (only dilution in water and filtering), (ii) high-throughput screening (24 injections h-1), (iii) proper recovery values (between 72 and 118%), and (iv) an inter-day precision of less than 7% for all analytes. The procedure was successfully applied in the analysis of seized cocaine samples collected by the Integrated Forensics Post (PPI) of the Minas Gerais Civil Police (Uberaba, Minas Gerais State, Brazil), during the year of 2018.


Subject(s)
Cocaine/analysis , High-Throughput Screening Assays , Illicit Drugs/analysis , Electric Conductivity , Electrophoresis, Capillary , Hydrogen-Ion Concentration
2.
J Sep Sci ; 40(8): 1815-1823, 2017 Apr.
Article in English | MEDLINE | ID: mdl-28217928

ABSTRACT

Paracetamol is an active ingredient commonly found in pharmaceutical formulations in combination with one of the following compounds: codeine, orphenadrine, promethazine, scopolamine, and tramadol. In this work, we propose a unique analytical method for determination of these active ingredients in pharmaceutical samples. The method is based on capillary electrophoresis with capacitively coupled contactless conductivity detection. The separation was achieved on a fused silica capillary (50 cm total length, 40 cm effective length, and 50 µm id) using an optimized background electrolyte composed of 20 mmol/L ß-alanine/4 mmol/L sodium chloride/4 µmol/L sodium hydroxide (pH 9.6). Each sample can be analyzed in a single run (≤2 min) and the limits of detection were 2.5, 0.62, 0.63, 2.5, 15, and 1.6 µmol/L for scopolamine, tramadol, orphenadrine, promethazine, codeine, and paracetamol, respectively. Recovery values for spiked samples were between 94 and 104%.


Subject(s)
Acetaminophen/analysis , Electrophoresis, Capillary , Codeine/analysis , Drug Compounding , Orphenadrine/analysis , Promethazine/analysis , Scopolamine/analysis , Tramadol/analysis
3.
J Chromatogr A ; 1472: 134-137, 2016 Nov 11.
Article in English | MEDLINE | ID: mdl-27773387

ABSTRACT

This paper reports for the first time, a method for simultaneous determination of naphazoline (NPZ) and zinc (Zn) using an analytical separation technique (capillary electrophoresis with capacitively coupled contactless conductivity detection -CE-C4D). A single run is possible every 55s (sampling rate=65h-1). The separation by CE-C4D was achieved on a fused silica capillary (50cm length - 10cm effective, 50µm i.d.) with a background electrolyte (BGE) composed by 20mmolL-1 of 2-(morpholin-4-yl)ethane-1-sulfonic acid (MES) and 20mmolL-1 of histidine (HIS) (pH 6.0). Detection limits were estimated at 20 and 30µmolL-1 and recovery values for spiked samples were 98 and 102% for NPZ and Zn, respectively. The developed procedure was compared to HPLC (NPZ) and FAAS (Zn) and no statistically significant differences were observed (95% confidence level).


Subject(s)
Electrophoresis, Capillary/methods , Naphazoline/analysis , Zinc/analysis , Chromatography, High Pressure Liquid , Electric Capacitance , Electric Conductivity , Electrolytes/chemistry , Limit of Detection
4.
J Sep Sci ; 38(10): 1657-62, 2015 May.
Article in English | MEDLINE | ID: mdl-25773878

ABSTRACT

Paracetamol, caffeine and ibuprofen are found in over-the-counter pharmaceutical formulations. In this work, we propose two new methods for simultaneous determination of paracetamol, caffeine and ibuprofen in pharmaceutical formulations. One method is based on high-performance liquid chromatography with diode-array detection and the other on capillary electrophoresis with capacitively coupled contactless conductivity detection. The separation by high-performance liquid chromatography with diode-array detection was achieved on a C18 column (250×4.6 mm(2), 5 µm) with a gradient mobile phase comprising 20-100% acetonitrile in 40 mmol L(-1) phosphate buffer pH 7.0. The separation by capillary electrophoresis with capacitively coupled contactless conductivity detection was achieved on a fused-silica capillary (40 cm length, 50 µm i.d.) using 10 mmol L(-1) 3,4-dimethoxycinnamate and 10 mmol L(-1) ß-alanine with pH adjustment to 10.4 with lithium hydroxide as background electrolyte. The determination of all three pharmaceuticals was carried out in 9.6 min by liquid chromatography and in 2.2 min by capillary electrophoresis. Detection limits for caffeine, paracetamol and ibuprofen were 4.4, 0.7, and 3.4 µmol L(-1) by liquid chromatography and 39, 32, and 49 µmol L(-1) by capillary electrophoresis, respectively. Recovery values for spiked samples were between 92-107% for both proposed methods.


Subject(s)
Acetaminophen/analysis , Caffeine/analysis , Chromatography, High Pressure Liquid/methods , Electrophoresis, Capillary/methods , Ibuprofen/analysis , Pharmaceutical Preparations/analysis , Spectrophotometry, Ultraviolet/methods
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