scholarly journals Performance comparison between solid phase extraction and magnetic carbon nanotubes facilitated dispersive-micro solid phase extractions (Mag-CNTs/d-µSPE) of a cyanide metabolite in biological samples using GC–MS

2021 ◽  
Vol 12 (1) ◽  
Author(s):  
Sun Yi Li ◽  
Ilona Petrikovics ◽  
Jorn Yu

AbstractDispersive-micro solid phase extraction (d-µSPE) has gained increasing attention due to its convenience, effectiveness, and flexibility for sorbent selection. Among a various selection of materials, magnetic carbon nanotubes (Mag-CNTs) is a promising d-µSPE sorbent with excellent separation efficiency in addition to its high surface area and adsorption capability. In this work, two different surface-modified Mag-CNTs, Mag-CNTs-COOH and Mag-CNTs-SO3H, were developed to facilitate d-µSPE (Mag-CNTs/d-µSPE). The cyanide metabolite, 2-aminothiazoline-4-carboxylic acid (ATCA), was selected to evaluate their extraction performance using gas chromatography–mass spectrometry (GC–MS) analysis. The Mag-CNTs-COOH enabled a one-step derivatization/desorption approach in the workflow; therefore, a better overall performance was achieved. Compared to the Mag-CNTs-SO3H/d-µSPE and SPE workflow, the one-step desorption/derivatization approach improved the overall extraction efficiency and reduced solvent consumption and waste production. Both Mag-CNTs/d-µSPE workflows were validated according to ANSI/ASB 036 guidelines and showed excellent analytical performances. The limit of detection (LOD) and limit of quantitation (LOQ) of ATCA in synthetic urine were 5 and 10 ng/mL, respectively, and that in bovine blood were achieved at 10 and 60 ng/mL. The SPE method’s LOD and LOQ were also determined at 1 and 25 ng/mL in bovine blood samples. The Mag-CNTs/d-µSPE methods demonstrated great potential to extract polar and ionic metabolites from biological matrices. The extraction processes of ATCA described in this work can provide an easier-to-adopt procedure for potential routine forensic testing of the stable biomarker in cyanide poisoning cases, particularly for those cases where the cyanide detection window has passed.

2019 ◽  
Vol 276 ◽  
pp. 458-466 ◽  
Author(s):  
Ainiyatul Nadiah Mohamad Nasir ◽  
Noorfatimah Yahaya ◽  
Nur Nadhirah Mohamad Zain ◽  
Vuanghao Lim ◽  
Sazlinda Kamaruzaman ◽  
...  

2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Paras P. Vekariya ◽  
Hitendra S. Joshi

Simple and rapid reverse phase high-performance liquid chromatography (RP-HPLC) method was developed and validated using solid phase extraction (SPE) technique for the determination of Azilsartan Medoxomil Potassium (AMP) in human plasma; detection was carried out by photo diode array detector. Chromatographic separation of the analyte AMP was achieved within 7.5 min by Waters symmetry C18 (4.6 × 250 mm, 5 µm) column, mobile phase was 25 mM ammonium acetate buffer (pH 5.5): acetonitrile 55 : 45 v/v, flow rate was 1.0 mL/min, and the detection was carried out at 254 nm. Calibration curve was linear (r2 > 0.9985) in the range of 1.0–9.0 µg/mL, limit of detection (LOD) and limit of quantitation (LOQ) were 0.150 µg/mL and 0.400 µg/mL, respectively, and intra- and interday deviations were between 1.53–8.41% and 1.78–4.59%, respectively. The overall mean recovery of AMP was 92.35%. No any endogenous constituents were found to interfere at retention time of the analyte. This new RP-HPLC method was successfully validated and may be applied to conduct bioavailability and bioequivalence studies of AMP.


2019 ◽  
Vol 7 (2) ◽  
pp. 245-253 ◽  
Author(s):  
Wan Norfazilah Wan Ismail ◽  
Dzul Iskandar Muhammad Fauzi ◽  
Nurlin Abu Samah

A rapid solid phase extraction (SPE) combined with gas chromatography equipped with mass spectrometry (GC-MS) method was developed and validated for the determination of acenaphthylene, acenaphthene and naphthalene in wastewater sample collected from petroleum industry’s drainage. Important SPE parameters, namely absorbent amount, sample volume, type of elution solvent and its volume were optimized. The optimum parameters obtained are: 200 mg silica nano-powder, 2.0 mL sample volume and 2.0 mL n-hexane as elution solvent. The method showed good linearity in the range of 0.1-10.0 mg/L with satisfactory limit of detection (≤1.0 mg/L) and limit of quantitation (≤3.2 mg/L) under the optimized conditions. Good relative recoveries (94.7-99.9%) and intra- and inter-day precisions (≤2.8%, n=3) for acenaphthene, acenaphthylene and naphthalene were obtained. Toxicity study has revealed that it is a non-toxic absorbent and safe to be used for the removal of organic pollutants in water which is advantageous for routine wastewater analysis.


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