Improved Solid-Phase Extraction Method for Systematic Toxicological Analysis in Biological Fluids

Soriano, T.; Jurado, Carmen; Menéndez, Manuel; Repetto, M.

doi:10.1093/jat/25.2.137

Cited by 52 publications

(34 citation statements)

References 19 publications

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“…The average within-day precision and accuracy of the proposed method as determined at 0.2 and 5 µg ml −1 (n = 10) in bile and vitreous humor are listed in Table 2. The results are similar to those reported by Vanbinst et al (2002), and lower than those obtained by Soriano et al (2001).…”

Section: Resultssupporting

confidence: 89%

GC-FID determination of cocaine and its metabolites in human bile and vitreous humor

et al. 2006

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Gas chromatography was used in combination with flame ionization detection (GC-FID) to develop a method for determining cocaine and its two metabolites, benzoylecgonine (BEG) and ecgonine methyl ester (EME), in bile and vitreous humor. The method used a 12 m x 0.2 mm i.d. column of 0.33 microm film thickness packed with 5% phenylmethylsiloxane, and proadifen as a reference compound. Drug-free bile and vitreous humor samples were used to prepare solutions of the target compounds at concentrations over the range 0.1-4 microg ml(-1) that were subjected to solid-phase extraction through Bond Elut Certify columns and derivatized with 99:1 (v/v) N,O-bis-trimethylsilyltrifluoroacetamide (BSTFA)/trimethylchlorosilane (TMCS). Calibration graphs were highly linear, with correlation coefficients above 0.99 in all instances. Also, the precision of the method was found to be quite acceptable, with coefficients of variation less than 5% for bile and less than 7% for vitreous humor. The average extraction yields ranged from 73.6% to 91.2% for bile and from 71.5% to 92.2% for vitreous humor. The proposed method was used to analyse 26 samples of bile and as many of vitreous humor from individuals fatally poisoned by cocaine, whether alone or in combination with other drugs. The mean drug levels found were 0.75 and 1.54 microg ml(-1) for cocaine in bile and vitreous humor, respectively, 6.35 and 0.94 microg ml(-1) for BEG, and 2.18 and 0.61 microg ml(-1) for EME.

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Section: Resultssupporting

confidence: 89%

GC-FID determination of cocaine and its metabolites in human bile and vitreous humor

et al. 2006

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“…In the preceding methods, the analysis took place on normal-phase chromatographic columns using more expensive, pollutant and toxic mobile phases, such as n-hexane:2-propanol, n-hexane:ethanol or n-hexane:ethanol:2-propanol. Besides the specific chromatographic conditions, the SPE procedure used here in sample pretreatment offers many other benefits over the traditional liquid-liquid extraction methods, such as faster sample preparation, lower cost, greater recoveries, less sample handling, improved safety and easy automation (Soriano et al, 2001;Camel, 2003). Even though ESL and its metabolites could be analyzed using MS detection systems (Hainzl et al, 2001;Almeida et al, 2005), most hospitals and laboratories are not equipped with such high-cost instruments (Velpandian et al, 2004;Janchawee et al, 2007).…”

Section: Discussionmentioning

confidence: 99%

Enantioselective HPLC‐UV method for determination of eslicarbazepine acetate (BIA 2‐093) and its metabolites in human plasma

Alves

Figueiredo

Castel‐Branco

et al. 2007

Biomedical Chromatography

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Determination of eslicarbazepine acetate ABSTRACT: Eslicarbazepine acetate (BIA 2-093) is a novel central nervous system drug undergoing clinical phase III trials for epilepsy and phase II trials for bipolar disorder. A simple and reliable chiral reversed-phase HPLC-UV method was developed and validated for the simultaneous determination of eslicarbazepine acetate, oxcarbazepine, S-licarbazepine and R-licarbazepine in human plasma. The analytes and internal standard were extracted from plasma by a solid-phase extraction using Waters Oasis ® HLB cartridges. Chromatographic separation was achieved by isocratic elution with water-methanol (88:12, v/v), at a flow rate of 0.7 mL/min, on a LichroCART 250-4 ChiraDex (β-cyclodextrin, 5 μm) column at 30°C. All compounds were detected at 225 nm. Calibration curves were linear over the range 0.4 -8 μg/mL for eslicarbazepine acetate and oxcarbazepine, and 0.4 -80 μg/ mL for each licarbazepine enantiomer. The overall intra-and interday precision and accuracy did not exceed 15%. Mean relative recoveries varied from 94.00 to 102.23% and the limit of quantification of the assay was 0.4 μg/mL for all compounds. This method seems to be a useful tool for clinical research and therapeutic drug monitoring of eslicarbazepine acetate and its metabolites S-licarbazepine, R-licarbazepine and oxcarbazepine.

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“…The sensitivity showed by our method using GC/MS was similar to that previously reported by using chromatographic methods. [15][16] Table 3 shows the results obtained for intra-assay and inter-assay precision calculations and selected ions used for qualification and quantification of all the analytes. Inter-day and intra-day precision were < 9.0% and <3.5% for all analytes.…”

Section: Resultsmentioning

confidence: 99%

Validation of a Method to Detect Central Nervous System Acting Drugs in Blood by Gc/Ms. Application in Cases of Death Caused by Phenothiazines in the North of Chile

Bravo

Ulloa

Venegas³

et al. 2014

J. Chil. Chem. Soc.

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A simple and rapid analytical method is developed and validated for the determination of antiepileptic and antipsychotic drugs in human whole blood using a solid-phase extraction and quantification by gas chromatography-mass spectrometry (GC/MS). Prazepam was used as internal standard (IS). The specificity, linearity, intra-and inter-assay precision and accuracy, and extraction recovery were fully evaluated. The limits of detection and quantification were in the range of 0.52 -0.98 mg/mL and 1.56 -2.97 mg/mL for antiepileptic drugs (pentobarbital, phenobarbital and carbamazepine) and 1.31 -2.94 ng/mL and 3.98 -8.89 ng/mL for antipsychotic drugs (chlorpromazine and thioridazine), respectively. The relative standard deviation (RSD) was less than 7.07%, while the intra-day accuracy was < 3.21% and the inter-day was < 8.80%, referred to RSD. The developed methodology was applied in forensic cases of death caused by phenothiazines in the North of Chile during 2010-2012.

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Improved Solid-Phase Extraction Method for Systematic Toxicological Analysis in Biological Fluids

Cited by 52 publications

References 19 publications

GC-FID determination of cocaine and its metabolites in human bile and vitreous humor

GC-FID determination of cocaine and its metabolites in human bile and vitreous humor

Enantioselective HPLC‐UV method for determination of eslicarbazepine acetate (BIA 2‐093) and its metabolites in human plasma

Validation of a Method to Detect Central Nervous System Acting Drugs in Blood by Gc/Ms. Application in Cases of Death Caused by Phenothiazines in the North of Chile

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