Automated hollow‐fiber liquid‐phase microextraction followed by liquid chromatography with mass spectrometry for the determination of benzodiazepine drugs in biological samples

Self Cite

An automated three-phase hollow fiber liquid-phase microextraction based on two immiscible organic solvents followed by high-performance liquid chromatography with UV-Vis detection method was applied for the extraction and determination of exemestane, letrozole, and paclitaxel in water and urine samples. n-Dodecane was selected as the supported liquid membrane and its polarity was justified by trioctylphosphine oxide. Acetonitrile was used as an organic acceptor phase with desirable immiscibility having n-dodecane. All the effective parameters of the microextraction procedure such as type of the organic acceptor phase, the supported liquid membrane composition, extraction time, pH of the donor phase, hollow fiber length, stirring rate, and ionic strength were evaluated and optimized separately by a one variable at-a-time method. Under the optimal conditions, the linear dynamic ranges were 1.8-200 (R = 0.9991), 0.9-200 (R = 0.9987) and 1.2-200 μg/L (R = 0.9983), and the limits of detection were 0.6, 0.3, and 0.4 μg/L for exemestane, letrozole, and paclitaxel, respectively. To evaluate the capability of the proposed method in the analysis of biological samples, three different urinary samples were analyzed under the optimal conditions. The relative recoveries of the three pharmaceuticals were in the range of 91-107.3% for these three analytes.

“…:

ER % = PF \times (\frac{V_{normala}}{V_{normals}}) \times 100

where V a and V s are the volumes of the acceptor phase and sample solution, respectively. Relative recovery (RR%) was calculated from the following equation:

RR % = \frac{C_{found} - C_{real}}{C_{added}} \times 100

Section: Methodsmentioning

confidence: 99%

Extraction and determination of trace amounts of three anticancer pharmaceuticals in urine by three‐phase hollow fiber liquid‐phase microextraction based on two immiscible organic solvents followed by high‐performance liquid chromatography

Nazaripour

Yamini

Bagheri

2018

Self Cite

“…However, continued use of BZPs may have adverse effects, such as drowsiness, dizziness, and decreased alertness. Furthermore, BZPs are readily available, which increases their potential for addiction . Besides, BZPs may also find their way into our environment, since they are excreted partially unchanged, and thus have been detected in wastewaters .…”

Section: Introductionmentioning

confidence: 99%

Fabrication of magnetic zinc adeninate metal–organic frameworks for the extraction of benzodiazepines from urine and wastewater

Zhang

Yao

Fu³

et al. 2018

In this study, an alternative method for synthesizing magnetic cobalt adeninate metal-organic frameworks was developed, and the synthesized materials were examined for their potential application for separating and enriching benzodiazepines from complex samples. Benzodiazepines, widely used as hypnotics, muscle relaxants, sedatives, and anxiolytics, are a class of drugs that require accurate detection and monitoring. Results showed that Fe O nanoparticles could be well anchored onto the external surface of cobalt adeninate metal-organic frameworks by using amino-silane as a linkage. Their adsorption of benzodiazepines was mainly promoted by intermolecular hydrogen binding, π-π interactions and electrostatic attraction. Their potential application was evaluated by extraction of benzodiazepines in urine and wastewater samples prior to liquid chromatography with mass spectrometry. Under optimum conditions, the calibration curves were linear with a correlation coefficient of ≥0.9928 in the concentration range of 10-5000 ng/L for lorazepam and 5-5000 ng/L for estazolam, chlordiazepoxide, alprazolam, midazolam and triazolam. The limits of detection were in the range of 0.71-2.49 ng/L. The percent of extraction recoveries were 80.2-94.5% for urine and 84.1-94.4% for wastewater, respectively. Results suggested that magnetic cobalt adeninate metal-organic frameworks could potentially be a promising material for enriching benzodiazepines from urine and wastewater with high accuracy and precision.

“…Analysis of classical BZDs is included in a systematic toxicology analysis (STA), when the first screening method is based on immunochemical tests and assays, and then followed by an instrumental analysis (LC–MS or GC–MS) for the confirmation and quantification of BZDs concentration levels in biological fluids (namely serum and urine) . Due to the structural similarity of the classical BZDs and DBZDs, the immunochemical screening can lead to positive results when DBZDs‐related metabolites (namely glucuronides) are present in the (urine) sample .…”

Section: Introductionmentioning

confidence: 99%

Analysis of selected designer benzodiazepines by ultra high performance liquid chromatography with high‐resolution time‐of‐flight mass spectrometry and the estimation of their partition coefficients by micellar electrokinetic chromatography

Tomková

Švidrnoch

Maier

et al. 2017

A new ultra high performance liquid chromatography with electrospray ionization time of flight mass spectrometry method for the selective and sensitive separation, identification, and determination of selected designer benzodiazepines (namely, pyrazolam, phenazepam, etizolam, flubromazepam, diclazepam, deschloroetizolam, bentazepam, nimetazepam, and flubromazolam) in human serum was developed. The separation of the studied designer benzodiazepines was achieved on C 18 chromatographic column using gradient elution within 6 min without any significant matrix interferences. Liquid-liquid extraction with butyl acetate was applied for serum samples cleanup and preconcentration of studied designer benzodiazepines. The method was validated in terms of linearity, limit of detection, limit of quantification, matrix effects, specificity, precision, accuracy, recovery, and sample stability. The limit of detection values were 0.10-0.15 ng/mL. The method was applied to a spiked serum sample to demonstrate its applicability for systematic toxicology analysis. Furthermore, a capillary chromatographic method with micellar electrokinetic chromatography was used for the estimation of partition coefficients of studied designer benzodiazepines as important parameters to evaluate their pharmacological and toxicological properties.