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Determination of cocaine adulterants in human urine by dispersive liquid-liquid microextraction and high-performance liquid chromatography

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Abstract

This study aimed to determine simultaneously five major street cocaine adulterants (caffeine, lidocaine, phenacetin, diltiazem, and hydroxyzine) in human urine by dispersive liquid-liquid microextraction (DLLME) and high-performance liquid chromatography. The chromatographic separation was obtained in gradient elution mode using methanol:water plus trifluoroacetic acid 0.15% (v/v) (pH = 1.9) at 1 mL min−1 as mobile phase, at 25 °C, detection at 235 nm, and analysis time of 20 min. The effect of major DLLME operating parameters on extraction efficiency was explored using the multifactorial experimental design approach. The optimum extraction condition was set as 4 mL human urine sample alkalized with 0.5 M sodium phosphate buffer (pH 12), NaCl (15%, m/v), 300 μL acetonitrile (dispersive solvent), and 800 μL chloroform (extraction solvent). Linear response (r2 ≥ 0.99) was obtained in the range of 180–1500 ng mL−1 with suitable selectivity, quantification limit (180 ng mL−1), mean recoveries (33.43–76.63%), and showing relative standard deviation and error (within and between-day assays) ≤15%. The analytes were stable after a freeze-thaw cycle and a short-term room temperature stability test. This method was successfully applied in real samples of cocaine users, suggesting that our study may contribute to the appropriate treatment of cocaine dependence or with the cases of cocaine acute intoxication.

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Acknowledgements

The authors thank CAPS-AD Eulâmpio Cordeiro, its members, and each person who provided the samples for this study. Additionally, the authors are grateful to CNPq (Brazilian National Council for Scientific and Technological Development) and FACEPE (State of Pernambuco Science and Technology Support Foundation) for granting a research fellowship.

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Authors and Affiliations

  1. Pharmaceutical Science Department, Federal University of Pernambuco, Prof. Artur de Sá S/N; Cidade Universitária, Recife, PE, 50740-521, Brazil

    Pedro Rafael da Silva, Rubens Pedro Lorena Silva, Danielle Cristine Almeida Silva de Santana & Fernando José Malagueño de Santana

  2. Laboratory of Forensic Toxicology, Criminalistics Institute, Secretary of Social Defense of Pernambuco, Marquês de Pombal 455, Santo Antônio, Recife, PE, 50100-170, Brazil

    Laís Cristina Santana Sena

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  1. Pedro Rafael da Silva
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da Silva, P.R., Sena, L.C.S., Silva, R.P.L. et al. Determination of cocaine adulterants in human urine by dispersive liquid-liquid microextraction and high-performance liquid chromatography. Anal Bioanal Chem 411, 3447–3461 (2019). https://doi.org/10.1007/s00216-019-01797-z

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