Targeted analysis of 116 drugs in hair by UHPLC‐MS/MS and its application to forensic cases

Abstract

A multi-target method that can detect a broad range of drugs in human hair, such as hypnotics, anxiolytics, analgesics, benzodiazepines, antihistamines, antidepressants, antipsychotics, and anticonvulsants, was developed based on ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The drugs were extracted from 10 mg of washed hair by incubation for 18 h in a 25:25:50 (v/v/v) mixture of methanol/acetonitrile/2 mM ammonium formate (8% acetonitrile, pH 5.3). For 51% of the basic drugs, the lower limits of quantification (LLOQs) were in the range of 0.05-0.5 pg/mg, and the majority (98%) were ≤ 5 pg/mg. Linearity ranged from LLOQs to 100-500 pg/mg for all the basic drugs. For acid and neutral drugs, the LLOQs ranged from 0.4 to 500 pg/mg, and linearity ranged from LLOQs to 80-40 000 pg/mg. According to published reports on concentrations attained in single dose control studies, the present method is sensitive enough to detect single-dose drug exposure for many of the drugs. The accuracy was within 75-125% for the majority of drugs. Good precision was observed (relative standard deviations [RSD%] < 25%) for most of the compounds, including the prepared quality control (QC) hair samples. The method was applied to forensic cases and concentrations of rarely reported drugs in hair in 25 post-mortem forensic cases were presented. Hair concentrations of amisulpride, gabapentin, mianserin, mepyramine, orphenadrine, and xylometazoline have not been previously reported. Copyright © 2016 John Wiley & Sons, Ltd.

Segmental analysis of antidepressant and antipsychotic drugs in the hair of schizophrenic patients

“…As shown in Table in this study, amisulpride was found in hair samples from two patients (9.2–20.3 ng/mg), aripiprazole and dehydroaripiprazole was detected in nine patients (250–730 ng/mg and 8.4–36.7 ng/mg, respectively), perphenazine was detected in five patients (0.02–0.19 ng/mg), olanzapine and norolanzapine was detected in five patients (<LOQ–1.44 ng/mg and <LOQ–0.12 ng/mg, respectively), and sulpiride was detected in two patients (19.5–125 ng/mg). The reported hair concentrations were higher in ours than in the published studies . This might be explained by the fact that fixed daily doses of medicines had been administered for a long period of time in the present study.…”

“…To the best of our knowledge, hair concentrations of amisulpride, aripiprazole, dehydroaripiprazole, perphenazine, olanzapine, norolanzapine, and sulpiride in hair have been scarcely reported, and the dose is rarely reported for patients or postmortem cases . As shown in Table in this study, amisulpride was found in hair samples from two patients (9.2–20.3 ng/mg), aripiprazole and dehydroaripiprazole was detected in nine patients (250–730 ng/mg and 8.4–36.7 ng/mg, respectively), perphenazine was detected in five patients (0.02–0.19 ng/mg), olanzapine and norolanzapine was detected in five patients (<LOQ–1.44 ng/mg and <LOQ–0.12 ng/mg, respectively), and sulpiride was detected in two patients (19.5–125 ng/mg).…”

“…As extraction solvents, methanol and EM (25:25:50 (v/v/v) mixture of methanol/acetonitrile/2 mM ammonium formate (8% acetonitrile, pH 5.3)) were compared. The results indicated that the extraction medium had a higher extraction efficiency and fewer matrix effects than methanol.…”

Different localizations of drugs simultaneously administered in a strand of hair by micro‐segmental analysis

“…Acetaminophen, acetyl salicylic acid, allyl isopropyl acetylurea, ibuprofen, isopropamide iodide, and the major metabolites of each of these drugs were either not detected from any hair segments or were only detected at low levels from some segments when all administered drugs were assessed in the preliminary study. It is known that acidic compounds are generally not taken up into hair as easily as basic compounds, which have high affinity for melanin in hair . Additionally, we previously reported that acidic and neutral compounds, such as acetaminophen, allyl isopropyl acetylurea, and ibuprofen were scarcely detected from hair in experiments that used bulk hair samples .…”

Surveillance of drug abuse in Hong Kong by hair analysis using LC‐MS/MS

“…In addition, hair collection is easy, non‐invasive and, is difficult to adulterate . Taking advantage of the high sensitivity of liquid chromatography–tandem mass spectrometry (LC–MS/MS) based method, hair drug testing by LC–MS/MS is a common approach in identifying drug exposure …”