• Journal of Korean Society of Environmental Engineers
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• v.35 no.2
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• pp.75-83
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• 2013

We applied a sensitive method based on on-line solid-phase extraction (SPE) and liquid chromatography/mass spectrometry (LC/MSD) using an electrospray interface for the determination of eleven perfluorinated compounds (PFCs) in water. The on-line connection suppressed the target loss by keeping the cartridge from drying, which resulted in improvement of the recovery and saving of the analytical time. For the on-line solid-phase extraction of 10 mL water samples, recoveries were between $80.4{\pm}5.2%{\sim}109.5{\pm}1.4%$ and limit of quantification (LOQ) were 3.6~15.9 ng/L for the PFCs. The total PFCs concentrations of the tributaries and main stream of Nakdong River water samples were in the range of $8.0{\sim}678.6{\mu}g/L$.

• Journal of Environmental Health Sciences
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• v.38 no.6
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• pp.561-567
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• 2012

Objectives: Parabens are widely used as antimicrobial agents in pharmaceuticals and cosmetics as well as by the food industry. Parabens have been reported to show weak estrogenic activity and be related to health effects such as allergic reactions and skin and breast cancer. We evaluated an online solid phase extraction (SPE) method coupled with LC-MS/MS technique using free and conjugated parent parabens in human urine for assessing human exposure to parabens. Methods: We employed LC/MS/MS through online solid phase extraction and column-switching techniques and analyzed free and conjugated parabens as biomarkers of human exposure. Four major parabens, methyl-paraben (MP), ethyl-paraben (EP), propyl-paraben (PP) and butyl-paraben (BP), were analyzed. Method validation was performed by sensitivity, accuracy, precision and comparison of the results of online SPE with offline SPE. Results: The limits of detection (LOD) were in the range of 0.2-2 ng/mL, and actual limits of quantification (LOQ) were in the range of 0.7-6 ng/mL urine, depending upon the compound. Accuracy was in the range of 98.3-106.4%, and precision was in the range of 1.3-8.7% (CV) depending upon the compound. We found a good correlation between the results of analysis by online SPE method and that by off-line SPE method. Conclusions: The online SPE method showed proper LOD and validated accuracy, precision and good correlation with the offline method for analyzing parabens in urine.

• Journal of Korean Society of Water and Wastewater
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• v.32 no.6
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• pp.559-572
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• 2018

The aim of this study was to evaluate pretreatment methods for 27 pharmaceuticals and personal care products (PPCPs) in various sewage samples using a modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) and online solid-phase extraction with LC-MS/MS. Extraction efficiencies of PPCPs in the solid phase under different experimental conditions were evaluated, showing that the highest recoveries were obtained with the addition of sodium sulfate and ethylenediaminetetraacetic acid disodium salt dehydrate in acidified conditions. The recoveries of target compounds ranged from 91 to 117.2% for liquid samples and from 61.3 to 137.2% for solid samples, with a good precision. The methods under development were applied to sewage samples collected in two sewage treatment plants (STPs) to determine PPCPs in liquid and solid phases. Out of 27 PPCPs, more than 19 compounds were detected in liquid samples (i.e., influent and effluent) of two STPs, with concentration ranges of LOQ-33,152 ng/L in influents and LOQ-4,523 ng/L in effluents, respectively. In addition, some PPCPs such as acetylsalicylic acid, ibuprofen, and ofloxacin were detected at high concentrations in activated sludge as well as in excess sludge. This methodology was successfully applied to sewage samples for the determination of the target compounds in STPs.

• Analytical Science and Technology
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• v.31 no.1
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• pp.39-46
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• 2018

Carbaryl and seven organophosphorous pesticides were analyzed simultaneously using on-line solid phase extraction (on-line SPE) coupled with liquid chromatography tandem mass spectrometry (LC/MS/MS). The target pesticides are Carbaryl, Methyl demeton, Fenitrothion, Malathion, Parathion, Phenthoate, Diazinon, and EPN. This method includes the direct injection of $500{\mu}L$ in the water sample, a 15 min separation period using a rapid resolution liquid chromatography system with on-line SPE, and detection through electrospray ionization (ESI) positive mode. The percentage of recovery of all pesticides ranged from 85.3 % to 100 %. This method showed an accuracy of ${\geq}90.0%$, possessing limits of detection and quantification within 0.05 to $0.28{\mu}g/L$ and 0.16 to $0.89{\mu}g/L$, respectively. The correlation coefficients (r) for the calibration curves within a range of 0.5 to $8.0{\mu}g/L$ were higher than 0.99. The evaluation results showed the efficacy of the method for all contents, and no pesticides were detected in the water quality sample.