Abstract
The study aims the development and validation of a LC-MS/MS method for the identification and quantification of benzodiazepines and zolpidem in nails as alternative keratinized matrix to hair in long-term monitoring of anxiolytic and hypnotic drugs. Both fingernail and toenail samples (1-2 mm) were collected by clipping the excess overhang of the nail from volunteers and from postmortem cases. They were washed twice with organic solvents, dried under nitrogen stream, pulverized, immersed in a methanol solution (internal standard: diazepam-D5) and sonicated up to two hours. The solution was then direct injected in the LC-MS/MS system. Mass spectrometry was set in MRM mode, selecting two transitions for each substance. 32 analytes among benzodiazepines, metabolites and hypnotics were included in the list. The method fulfilled the internationally required criteria for validation. Limits of detection ranged from 0.03 pg/mg (zolpidem) to 13.1 pg/mg (bromazepam). 9 subjects under therapy were positive at 7 different benzodiazepines and/or metabolites (lorazepam, desalkylflurazepam, bromazepam, diazepam, alprazolam, lormetazepam and prazepam), while 5 molecules were measured in 4 postmortem cases (diazepam, desmethyldiazepam, delorazepam, 7-aminoclonazepam and zolpidem). In vitro experiments on eight authentic samples suggested that benzodiazepines in nails are influenced by the prolonged exposure to chlorinated water.
| Original language | English |
|---|---|
| Pages (from-to) | 137-142 |
| Number of pages | 6 |
| Journal | Journal of Pharmaceutical and Biomedical Analysis |
| Volume | 152 |
| DOIs | |
| Publication status | Published - Apr 15 2018 |
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Keywords
- Benzodiazepines/chemistry
- Bromazepam/chemistry
- Chlorine/adverse effects
- Chromatography, Liquid/methods
- Diazepam/chemistry
- Female
- Forensic Toxicology/methods
- Humans
- Limit of Detection
- Male
- Nails/chemistry
- Pyridines/chemistry
- Tandem Mass Spectrometry/methods
- Water/adverse effects
- Zolpidem
Cite this
Evaluation of benzodiazepines and zolpidem in nails and their stability after prolonged exposure to chlorinated water. / Moretti, Matteo; Andrello, Luisa; Visonà, Silvia; Vignali, Claudia; Groppi, Angelo; Freni, Francesca; Osculati, Antonio; Tajana, Luca; Morini, Luca.
In: Journal of Pharmaceutical and Biomedical Analysis, Vol. 152, 15.04.2018, p. 137-142.Research output: Contribution to journal › Article
}
TY - JOUR
T1 - Evaluation of benzodiazepines and zolpidem in nails and their stability after prolonged exposure to chlorinated water
AU - Moretti, Matteo
AU - Andrello, Luisa
AU - Visonà, Silvia
AU - Vignali, Claudia
AU - Groppi, Angelo
AU - Freni, Francesca
AU - Osculati, Antonio
AU - Tajana, Luca
AU - Morini, Luca
N1 - Copyright © 2018 Elsevier B.V. All rights reserved.
PY - 2018/4/15
Y1 - 2018/4/15
N2 - The study aims the development and validation of a LC-MS/MS method for the identification and quantification of benzodiazepines and zolpidem in nails as alternative keratinized matrix to hair in long-term monitoring of anxiolytic and hypnotic drugs. Both fingernail and toenail samples (1-2 mm) were collected by clipping the excess overhang of the nail from volunteers and from postmortem cases. They were washed twice with organic solvents, dried under nitrogen stream, pulverized, immersed in a methanol solution (internal standard: diazepam-D5) and sonicated up to two hours. The solution was then direct injected in the LC-MS/MS system. Mass spectrometry was set in MRM mode, selecting two transitions for each substance. 32 analytes among benzodiazepines, metabolites and hypnotics were included in the list. The method fulfilled the internationally required criteria for validation. Limits of detection ranged from 0.03 pg/mg (zolpidem) to 13.1 pg/mg (bromazepam). 9 subjects under therapy were positive at 7 different benzodiazepines and/or metabolites (lorazepam, desalkylflurazepam, bromazepam, diazepam, alprazolam, lormetazepam and prazepam), while 5 molecules were measured in 4 postmortem cases (diazepam, desmethyldiazepam, delorazepam, 7-aminoclonazepam and zolpidem). In vitro experiments on eight authentic samples suggested that benzodiazepines in nails are influenced by the prolonged exposure to chlorinated water.
AB - The study aims the development and validation of a LC-MS/MS method for the identification and quantification of benzodiazepines and zolpidem in nails as alternative keratinized matrix to hair in long-term monitoring of anxiolytic and hypnotic drugs. Both fingernail and toenail samples (1-2 mm) were collected by clipping the excess overhang of the nail from volunteers and from postmortem cases. They were washed twice with organic solvents, dried under nitrogen stream, pulverized, immersed in a methanol solution (internal standard: diazepam-D5) and sonicated up to two hours. The solution was then direct injected in the LC-MS/MS system. Mass spectrometry was set in MRM mode, selecting two transitions for each substance. 32 analytes among benzodiazepines, metabolites and hypnotics were included in the list. The method fulfilled the internationally required criteria for validation. Limits of detection ranged from 0.03 pg/mg (zolpidem) to 13.1 pg/mg (bromazepam). 9 subjects under therapy were positive at 7 different benzodiazepines and/or metabolites (lorazepam, desalkylflurazepam, bromazepam, diazepam, alprazolam, lormetazepam and prazepam), while 5 molecules were measured in 4 postmortem cases (diazepam, desmethyldiazepam, delorazepam, 7-aminoclonazepam and zolpidem). In vitro experiments on eight authentic samples suggested that benzodiazepines in nails are influenced by the prolonged exposure to chlorinated water.
KW - Benzodiazepines/chemistry
KW - Bromazepam/chemistry
KW - Chlorine/adverse effects
KW - Chromatography, Liquid/methods
KW - Diazepam/chemistry
KW - Female
KW - Forensic Toxicology/methods
KW - Humans
KW - Limit of Detection
KW - Male
KW - Nails/chemistry
KW - Pyridines/chemistry
KW - Tandem Mass Spectrometry/methods
KW - Water/adverse effects
KW - Zolpidem
U2 - 10.1016/j.jpba.2018.01.051
DO - 10.1016/j.jpba.2018.01.051
M3 - Article
C2 - 29414005
VL - 152
SP - 137
EP - 142
JO - Journal of Pharmaceutical and Biomedical Analysis
JF - Journal of Pharmaceutical and Biomedical Analysis
SN - 0731-7085
ER -