Comparison of different solid-phase extraction materials for sample preparation in the analysis of veterinary drugs in water samples

Mutavdžić, Dragana; Babić, Sandra; Ašperger, Danijela; Horvat, Alka J.M.; Kaštelan‐Macan, Marija

doi:10.1556/jpc.19.2006.6.9

Cited by 9 publications

(7 citation statements)

References 33 publications

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“…The pharmaceuticals were extracted from the water samples and preconcentrated on different 200 and 500 mg types of cartridges (Strata‐X, Strata‐X‐C, Strata C18‐E, Strata C8 and Strata SDB‐L) using methanol as an eluent 20 on the apparatus for SPE (Supelco, Bellefonte, USA). Before applying the spiked water samples, the cartridges were conditioned with 5 mL of methanol and water (pH 4.0) 20. A sample volume of 100 mL was applied to the cartridge and the flow was kept at no greater than 4 mL/min.…”

Section: Methodsmentioning

confidence: 99%

“…After the vacuum drying period of the sorbent, the loaded cartridges were eluted with methanol (eight volume of sorbent bed). Following the elution, the filtrates were evaporated on a rotary evaporator at 40 °C to dryness and the residues were dissolved in 1 mL of methanol to obtain a 100‐fold preconcentration 14, 20.…”

Section: Methodsmentioning

confidence: 99%

“…Before applying the spiked water samples, the cartridges were conditioned with 5 mL of methanol and water (pH 4.0) [20]. A sample volume of 100 mL was applied to the cartridge and the flow was kept at no greater than 4 mL/min.…”

Section: Spe Extraction and Hplc-dad Analysismentioning

confidence: 99%

“…Consequently, in this work, with regard to Oasis HLB, several SPE cartridges donated from Phenomenex and Vita Lab Nova d.o.o., Croatia have been compared and evaluated. This was performed under the same extraction conditions (pH 4.0 and methanol) [14,20] with the goal of efficiently extracting all the pharmaceuticals investigated, as well as achieving better recovery of SGUA. The five tested SPE cartridges contained the same amount of sorbent (500 mg) but differed in their nature and specific surface area ( Table 2).…”

Section: Selection Of the Spe Type Of Sorbentmentioning

confidence: 99%

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Development and optimization of the SPE procedure for determination of pharmaceuticals in water samples by HPLC‐diode array detection

Pavlović

Babić

Dolar

et al. 2010

J of Separation Science

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This paper focuses on the investigation of different types of SPE sorbents for the preconcentration of eight veterinary pharmaceuticals from water samples. The pharmaceuticals studied were sulfamethazine, sulfadiazine, sulfaguanidine, trimethoprim, oxytetracycline, enrofloxacin, norfloxacin and penicillin G/procaine. Five different SPE materials (Strata-X, Strata-X-C, Strata SDB-L, Strata C8 and Strata C18) from Phenomenex were compared with Oasis HLB with a view to obtaining the best cartridges for all pharmaceuticals investigated. Extraction efficiency was determined by HPLC with diode array detection (DAD). HPLC-DAD separation and quantification of the selected pharmaceuticals were carried out under gradient elution by a binary mixture of 0.01 M oxalic acid and ACN based on cyano modified column (LiChrosphere 100 CN) from Merck. Strata-X provided the best results in the preconcentration of 100 mL water samples, yielding average pharmaceutical recoveries of higher than 90%, except for sulfaguanidine (76.1%). The developed Strata-X-HLPC-DAD method was validated and applied, for the efficient investigation of reverse osmosis/nanofiltration membranes and for the removal of these eight pharmaceuticals from the production wastewater samples. NF90 and XLE membranes were shown to be the best for the rejection of all investigated pharmaceuticals.

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Section: Methodsmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

Section: Spe Extraction and Hplc-dad Analysismentioning

confidence: 99%

Section: Selection Of the Spe Type Of Sorbentmentioning

confidence: 99%

See 2 more Smart Citations

Development and optimization of the SPE procedure for determination of pharmaceuticals in water samples by HPLC‐diode array detection

Pavlović

Babić

Dolar

et al. 2010

J of Separation Science

Self Cite

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“…During the evaporation at 40°C, diethylene glycol in acetone, a keeper solution, was added to each sample to prevent some volatile pesticides from evaporating with the solvent [17]. To maintain the optimal and rugged performance of the florisil SPE, the sorbent was prevented from drying out during the conditioning, sample loading, and elution steps, as described by Mutavdžić et al [18].…”

Section: Recovery Without N-hexane/acetonitrile Partitioning (Non-parmentioning

confidence: 99%

A simultaneous multiresidue analysis for 203 pesticides in soybean using florisil solid-phase extraction and gas chromatography–tandem mass spectrometry

2018

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A multiresidue analysis method for the simultaneous determination of 203 pesticides in soybean was developed using solid-phase extraction (SPE) and gas chromatography-tandem mass spectrometry (GC-MS/ MS). Scheduled multiple reaction monitoring by GC-MS/ MS was optimized in electron ionization mode. The target pesticides satisfied the method limit of quantitation below 0.01 mg/kg, and an excellent instrumental repeatability was obtained. The calibration curve correlation coefficients (r 2) for 201 (99.0%) pesticides were C 0.990. The Multiclass Pesticide Multiresidue Method (No. 2) of the Korea Food Code was scaled down and applied for efficient sample treatment. Soybean sample (10 g) was extracted with 20 mL acetonitrile. The sample was filtered, partitioned with sodium chloride, and centrifuged. The supernatant (8 mL) was subjected to cleanup with a florisil SPE cartridge (500 mg), and the final extract was subjected to GC-MS/MS analysis. To remove fat, further liquid-liquid partitioning with n-hexane/acetonitrile was conducted before the SPE cleanup, and this procedure was compared to the non-partitioning procedure. The percentage of pesticides satisfying the recovery range of 70-120% with a relative standard deviation B 20% in the non-partitioning and partitioning procedures were 87.2% and 78.8% at 0.01 mg/kg and 88.2% and 76.8% at 0.05 mg/kg, respectively. The average matrix effect value (%) was 5.5%. This miniaturized analytical method can be successfully applied for rapid and sensitive monitoring of multiresidues in soybean and related agricultural products.

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Determination of multi-class pharmaceuticals in wastewater by liquid chromatography–tandem mass spectrometry (LC–MS–MS)

et al. 2010

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An analytical method for multi-class pharmaceuticals determination in wastewater has been developed and validated. Target compounds were: sulfonamides (sulfadiazine, sulfaguanidine, sulfamethazine, sulfamethoxazole), fluoroquinolones (ciprofloxacin, enrofloxacin, norfloxacin), diaminopyrimidine (trimethoprim), anaesthetic (procaine), anthelmintic (praziquantel and febantel), and macrolide (roxithromycin). The method involves pre-concentration and clean-up by solid-phase extraction (SPE) using Strata-X extraction cartridges at pH 4.0. Target analytes were identified and quantitatively determined by liquid chromatography-tandem mass spectrometry using multiple reaction monitoring (MRM). Recoveries were higher than 50% with relative standard deviation (RSD) below 18.3% for three concentrations. Only for sulfaguanidine was low recovery obtained. Matrix effect was evaluated using matrix-matched standards. The method detection limit (MDL) was between 0.5 and 5 ng L(-1) in spiked water samples. The precision of the method, calculated as relative standard deviation, ranged from 0.5 to 2.0% and from 1.4 to 8.3 for intra-day and inter-day analysis, respectively. The described analytical method was used for determination of pharmaceuticals in effluent wastewaters from the pharmaceutical industry.

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Comparison of different solid-phase extraction materials for sample preparation in the analysis of veterinary drugs in water samples

Cited by 9 publications

References 33 publications

Development and optimization of the SPE procedure for determination of pharmaceuticals in water samples by HPLC‐diode array detection

Development and optimization of the SPE procedure for determination of pharmaceuticals in water samples by HPLC‐diode array detection

A simultaneous multiresidue analysis for 203 pesticides in soybean using florisil solid-phase extraction and gas chromatography–tandem mass spectrometry

Determination of multi-class pharmaceuticals in wastewater by liquid chromatography–tandem mass spectrometry (LC–MS–MS)

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