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Gas chromatographic determination of cocaine and its metabolites in blood and urine from cocaine users in northwestern Spain

A gas chromatographic method with flame ionization detection (GC/FID) was developed for the determination of cocaine and its metabolites in blood and urine samples from cocaine users in Northwestern Spain. After a solid‐phase extraction with Bond Elut Certify cartridges and a derivatization with bis‐...

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Published in:Journal of applied toxicology 2004-07, Vol.24 (4), p.283-287
Main Authors: Fernández, P., Buján, L., Bermejo, A. M., Tabernero, M. J.
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description A gas chromatographic method with flame ionization detection (GC/FID) was developed for the determination of cocaine and its metabolites in blood and urine samples from cocaine users in Northwestern Spain. After a solid‐phase extraction with Bond Elut Certify cartridges and a derivatization with bis‐trimethylsilyltrifluoroacetamide–trimethylchlorosilane (1%), calibration curves were constructed over 0.4–4 µg ml−1 for urine and 0.1–2 µg ml−1 for blood, using proadifen as the reference compound. The average extraction recoveries were 75% for urine and 78% for blood. The limits of detection and quantitation were 0.071 and 0.24 µg ml−1, respectively. Coefficients of variation were
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M. ; Tabernero, M. J.</creator><creatorcontrib>Fernández, P. ; Buján, L. ; Bermejo, A. M. ; Tabernero, M. J.</creatorcontrib><description>A gas chromatographic method with flame ionization detection (GC/FID) was developed for the determination of cocaine and its metabolites in blood and urine samples from cocaine users in Northwestern Spain. After a solid‐phase extraction with Bond Elut Certify cartridges and a derivatization with bis‐trimethylsilyltrifluoroacetamide–trimethylchlorosilane (1%), calibration curves were constructed over 0.4–4 µg ml−1 for urine and 0.1–2 µg ml−1 for blood, using proadifen as the reference compound. The average extraction recoveries were 75% for urine and 78% for blood. The limits of detection and quantitation were 0.071 and 0.24 µg ml−1, respectively. Coefficients of variation were &lt;10% and accuracy was within ±12%. The average blood concentrations of cocaine, benzoylecgonine and ecgonine methyl ester in 42 living patients were 0.22, 1.43 and 0.16 µg ml−1, respectively. Urine samples were collected from individuals in the criminal justice system (70 cases), from drug abusers admitted to emergency rooms (36 cases) and from patients under detoxification treatment (36 cases). The second group exhibited the highest average concentrations (e.g. 0.97 µg ml−1 for cocaine, 5.23 µg ml−1 for benzoylecgonine and 0.39 µg ml−1 for ecgonine methyl ester). Sixty‐five fatal intoxications due to cocaine alone or in combination with other drugs were studied, and average blood levels were found to be higher in the deaths related to cocaine alone (e.g. 0.40 µg ml−1 for cocaine, 2.38 µg ml−1 for benzoylecgonine and 0.38 µg ml−1 for ecgonine methyl ester). 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M.</creatorcontrib><creatorcontrib>Tabernero, M. J.</creatorcontrib><title>Gas chromatographic determination of cocaine and its metabolites in blood and urine from cocaine users in northwestern Spain</title><title>Journal of applied toxicology</title><addtitle>J. Appl. Toxicol</addtitle><description>A gas chromatographic method with flame ionization detection (GC/FID) was developed for the determination of cocaine and its metabolites in blood and urine samples from cocaine users in Northwestern Spain. After a solid‐phase extraction with Bond Elut Certify cartridges and a derivatization with bis‐trimethylsilyltrifluoroacetamide–trimethylchlorosilane (1%), calibration curves were constructed over 0.4–4 µg ml−1 for urine and 0.1–2 µg ml−1 for blood, using proadifen as the reference compound. The average extraction recoveries were 75% for urine and 78% for blood. The limits of detection and quantitation were 0.071 and 0.24 µg ml−1, respectively. Coefficients of variation were &lt;10% and accuracy was within ±12%. The average blood concentrations of cocaine, benzoylecgonine and ecgonine methyl ester in 42 living patients were 0.22, 1.43 and 0.16 µg ml−1, respectively. Urine samples were collected from individuals in the criminal justice system (70 cases), from drug abusers admitted to emergency rooms (36 cases) and from patients under detoxification treatment (36 cases). The second group exhibited the highest average concentrations (e.g. 0.97 µg ml−1 for cocaine, 5.23 µg ml−1 for benzoylecgonine and 0.39 µg ml−1 for ecgonine methyl ester). Sixty‐five fatal intoxications due to cocaine alone or in combination with other drugs were studied, and average blood levels were found to be higher in the deaths related to cocaine alone (e.g. 0.40 µg ml−1 for cocaine, 2.38 µg ml−1 for benzoylecgonine and 0.38 µg ml−1 for ecgonine methyl ester). 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Psychiatry</subject><subject>Psychopharmacology</subject><subject>Sensitivity and Specificity</subject><subject>solid-phase extraction</subject><subject>Spain - epidemiology</subject><subject>Substance Abuse Detection - methods</subject><subject>Toxicology</subject><subject>urine</subject><issn>0260-437X</issn><issn>1099-1263</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2004</creationdate><recordtype>article</recordtype><recordid>eNp10E1v1DAQBmALgei2IP4B8oX2gFLGsfPhY1XaBbQqAorKzZo4NuuSxIudqFTqj6-3WbUnTj7MM-9YLyFvGBwzgPzDNY7HUopnZMFAyozlJX9OFpCXkAle_doj-zFeA6RZXr8ke6zgABUrF-RuiZHqdfA9jv53wM3aadqa0YTeDTg6P1BvqfYa3WAoDi11Y6S9GbHxnRtNpG6gTed9-zCcwpbZFPe4M0UTHtTgw7i-MTFlD_THJg1fkRcWu2he794D8vP87PL0U7b6uvx8erLKtGC5yKpKG82NLAshW6iNbbDOhagsb1gtrSx1DlxoKSpd5qyuEVu2NWi5ZI0W_IAczrmb4P9O6Qeqd1GbrsPB-CkqVhUgcqgTPJqhDj7GYKzaBNdjuFUM1LZolYpWqegk3-4ip6Y37ZPbNZvAux3AqLGzAQft4pMrAeqigOTez-7Gdeb2f_fUl5PL-Ww2a5dq_PeoMfxRZcWrQl1dLNX3FVx8XJbf1BW_B9rRpO8</recordid><startdate>200407</startdate><enddate>200407</enddate><creator>Fernández, P.</creator><creator>Buján, L.</creator><creator>Bermejo, A. 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Toxicol</addtitle><date>2004-07</date><risdate>2004</risdate><volume>24</volume><issue>4</issue><spage>283</spage><epage>287</epage><pages>283-287</pages><issn>0260-437X</issn><eissn>1099-1263</eissn><coden>JJATDK</coden><abstract>A gas chromatographic method with flame ionization detection (GC/FID) was developed for the determination of cocaine and its metabolites in blood and urine samples from cocaine users in Northwestern Spain. After a solid‐phase extraction with Bond Elut Certify cartridges and a derivatization with bis‐trimethylsilyltrifluoroacetamide–trimethylchlorosilane (1%), calibration curves were constructed over 0.4–4 µg ml−1 for urine and 0.1–2 µg ml−1 for blood, using proadifen as the reference compound. The average extraction recoveries were 75% for urine and 78% for blood. The limits of detection and quantitation were 0.071 and 0.24 µg ml−1, respectively. Coefficients of variation were &lt;10% and accuracy was within ±12%. The average blood concentrations of cocaine, benzoylecgonine and ecgonine methyl ester in 42 living patients were 0.22, 1.43 and 0.16 µg ml−1, respectively. Urine samples were collected from individuals in the criminal justice system (70 cases), from drug abusers admitted to emergency rooms (36 cases) and from patients under detoxification treatment (36 cases). The second group exhibited the highest average concentrations (e.g. 0.97 µg ml−1 for cocaine, 5.23 µg ml−1 for benzoylecgonine and 0.39 µg ml−1 for ecgonine methyl ester). Sixty‐five fatal intoxications due to cocaine alone or in combination with other drugs were studied, and average blood levels were found to be higher in the deaths related to cocaine alone (e.g. 0.40 µg ml−1 for cocaine, 2.38 µg ml−1 for benzoylecgonine and 0.38 µg ml−1 for ecgonine methyl ester). 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subjects benzoylecgonine
Biological and medical sciences
blood
cocaine
Cocaine - blood
Cocaine - metabolism
Cocaine - urine
Cocaine-Related Disorders - blood
Cocaine-Related Disorders - diagnosis
Cocaine-Related Disorders - mortality
Cocaine-Related Disorders - urine
derivatization
Drug addictions
ecgonine methyl ester
Female
Flame Ionization
GC/FID
General aspects. Methods
Humans
intoxications
Male
Medical sciences
Neuropharmacology
Pharmacology. Drug treatments
Psychoanaleptics: cns stimulant, antidepressant agent, nootropic agent, mood stabilizer..., (alzheimer disease)
Psychology. Psychoanalysis. Psychiatry
Psychopharmacology
Sensitivity and Specificity
solid-phase extraction
Spain - epidemiology
Substance Abuse Detection - methods
Toxicology
urine
title Gas chromatographic determination of cocaine and its metabolites in blood and urine from cocaine users in northwestern Spain
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