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 in | Analytical and bioanalytical chemistry Vol. 411; no. 16; pp. 3447 - 3461 |
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Main Authors | , , , , |
Format | Journal Article |
Language | English |
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. |
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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 |
Author_xml | – sequence: 1 givenname: Pedro Rafael surname: da Silva fullname: da Silva, Pedro Rafael organization: Pharmaceutical Science Department, Federal University of Pernambuco – sequence: 2 givenname: Laís Cristina Santana surname: Sena fullname: Sena, Laís Cristina Santana organization: Laboratory of Forensic Toxicology, Criminalistics Institute, Secretary of Social Defense of Pernambuco – sequence: 3 givenname: Rubens Pedro Lorena surname: Silva fullname: Silva, Rubens Pedro Lorena organization: Pharmaceutical Science Department, Federal University of Pernambuco – sequence: 4 givenname: Danielle Cristine Almeida Silva surname: de Santana fullname: de Santana, Danielle Cristine Almeida Silva organization: Pharmaceutical Science Department, Federal University of Pernambuco – sequence: 5 givenname: Fernando José Malagueño surname: de Santana fullname: de Santana, Fernando José Malagueño email: fmalagueno@hotmail.com organization: Pharmaceutical Science Department, Federal University of Pernambuco |
BackLink | https://www.ncbi.nlm.nih.gov/pubmed/31123783$$D View this record in MEDLINE/PubMed |
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CitedBy_id | crossref_primary_10_1016_j_ijoes_2023_100134 crossref_primary_10_4155_bio_2021_0237 crossref_primary_10_1016_j_microc_2020_105332 crossref_primary_10_1039_D1AY00932J crossref_primary_10_1039_D1AN01173A crossref_primary_10_1007_s13738_022_02642_4 crossref_primary_10_1016_j_chroma_2021_462444 crossref_primary_10_1080_03067319_2021_2014473 crossref_primary_10_1002_wfs2_1497 crossref_primary_10_1016_j_talo_2021_100079 crossref_primary_10_1016_j_forc_2024_100554 crossref_primary_10_3390_toxins13110793 |
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Copyright | Springer-Verlag GmbH Germany, part of Springer Nature 2019 COPYRIGHT 2019 Springer Analytical and Bioanalytical Chemistry is a copyright of Springer, (2019). All Rights Reserved. |
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Keywords | Dispersive liquid-liquid microextraction Urine drug testing Liquid chromatography Street cocaine Drug adulteration |
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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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