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

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...

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Published inAnalytical and bioanalytical chemistry Vol. 411; no. 16; pp. 3447 - 3461
Main Authors da Silva, Pedro Rafael, Sena, Laís Cristina Santana, Silva, Rubens Pedro Lorena, de Santana, Danielle Cristine Almeida Silva, de Santana, Fernando José Malagueño
Format Journal Article
LanguageEnglish
Published Berlin/Heidelberg Springer Berlin Heidelberg 01.06.2019
Springer
Springer Nature B.V
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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 ( r 2  ≥ 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.
AbstractList 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 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 (r  ≥ 0.99) was obtained in the range of 180-1500 ng mL with suitable selectivity, quantification limit (180 ng mL ), 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.
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.
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.sup.-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 [mu]L acetonitrile (dispersive solvent), and 800 [mu]L chloroform (extraction solvent). Linear response (r.sup.2 [greater than or equal to] 0.99) was obtained in the range of 180-1500 ng mL.sup.-1 with suitable selectivity, quantification limit (180 ng mL.sup.-1), mean recoveries (33.43-76.63%), and showing relative standard deviation and error (within and between-day assays) [less than or equal to]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.
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 ( r 2  ≥ 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.
Audience Academic
Author de Santana, Fernando José Malagueño
Sena, Laís Cristina Santana
da Silva, Pedro Rafael
Silva, Rubens Pedro Lorena
de Santana, Danielle Cristine Almeida Silva
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BackLink https://www.ncbi.nlm.nih.gov/pubmed/31123783$$D View this record in MEDLINE/PubMed
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Issue 16
Keywords Dispersive liquid-liquid microextraction
Urine drug testing
Liquid chromatography
Street cocaine
Drug adulteration
Language English
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– name: Heidelberg
PublicationTitle Analytical and bioanalytical chemistry
PublicationTitleAbbrev Anal Bioanal Chem
PublicationTitleAlternate Anal Bioanal Chem
PublicationYear 2019
Publisher Springer Berlin Heidelberg
Springer
Springer Nature B.V
Publisher_xml – name: Springer Berlin Heidelberg
– name: Springer
– name: Springer Nature B.V
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Snippet This study aimed to determine simultaneously five major street cocaine adulterants (caffeine, lidocaine, phenacetin, diltiazem, and hydroxyzine) in human urine...
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SubjectTerms Acetanilide
Acetonitrile
Acute intoxication
Adulterants
Alkalizing
Analytical Chemistry
Biochemistry
Caffeine
Characterization and Evaluation of Materials
Chemical properties
Chemistry
Chemistry and Materials Science
Chloroform
Chromatography
Cocaine
Dependence
Design of experiments
Diltiazem
Dispersion
Drug abuse
Elution
Experimental design
Extraction (Chemistry)
Food Science
Freeze thaw cycles
Freeze-thawing
High performance liquid chromatography
Human wastes
Identification and classification
Intoxication
Ions
Laboratory Medicine
Lidocaine
Liquid chromatography
Liquid-liquid extraction
Methods
Monitoring/Environmental Analysis
pH effects
Phenacetin
Research Paper
Selectivity
Sodium chloride
Sodium phosphate
Solvents
Stability tests
Trifluoroacetic acid
Urine
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Title Determination of cocaine adulterants in human urine by dispersive liquid-liquid microextraction and high-performance liquid chromatography
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