Ultrasound-assisted low-density solvent dispersive liquid–liquid microextraction for the determination of 4 designer benzodiazepines in urine samples by gas chromatography–triple quadrupole mass spectrometry

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Journal Article
Journal of Chromatography B: Analytical Technologies in the Biomedical and Life Sciences, 2017, 1053 pp. 9 - 15
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© 2017 Elsevier B.V. A novel microextraction technique based on ultrasound-assisted low-density solvent dispersive liquid–liquid microextraction (UA-LDS-DLLME) had been applied for the determination of 4 designer benzodiazepines (phenazepam, diclazepam, flubromazepam and etizolam) in urine samples by gas chromatography- triple quadrupole mass spectrometry (GC-QQQ-MS). Ethyl acetate (168 μL) was added into the urine samples after adjusting pH to 11.3. The samples were sonicated in an ultrasonic bath for 5.5 min to form a cloudy suspension. After centrifugation at 10000 rpm for 3 min, the supernatant extractant was withdrawn and injected into the GC-QQQ-MS for analysis. Parameters affecting the extraction efficiency have been investigated and optimized by means of single factor experiment and response surface methodology (Box-Behnken design). Under the optimum extraction conditions, a recovery of 73.8–85.5% were obtained for all analytes. The analytical method was linear for all analytes in the range from 0.003 to 10 μg/mL with the correlation coefficient ranging from 0.9978 to 0.9990. The LODs were estimated to be 1–3 ng/mL. The accuracy (expressed as mean relative error MRE) was within ±5.8% and the precision (expressed as relative standard error RSD) was less than 5.9%. UA-LDS-DLLME technique has the advantages of shorter extraction time and is suitable for simultaneous pretreatment of samples in batches. The combination of UA-LDS-DLLME with GC–QQQ–MS offers an alternative analytical approach for the sensitive detection of these designer benzodiazepines in urine matrix for clinical and medico-legal purposes.
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