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J Korean Soc Environ Eng > Volume 41(10); 2019 > Article
J Korean Soc Environ Eng 2019;41(10): 572-581. doi: https://doi.org/10.4491/KSEE.2019.41.10.572
고체상추출법과 GC/MS를 이용한 수질 환경 시료 중 아크릴아마이드 분석방법 연구
유대영1, 서하늘2, 장철현3
1한밭대학교 환경공학과
2(주)비앤지 기업부설연구소
3한밭대학교 건설환경공학과
Determination of Acrylamide in Aquatic Environmental Samples by GC/MS
Dae-Young Yu1, Ha-Neul Seo2, Cheol-Hyeon Chang3
1Department of Environmental Engineering, Hanbat National University
2B&G., R&D Center
3Department of Civil and Environmental Engineering, Hanbat National University
Corresponding author  Dae-Young Yu ,Tel: 042-255-6466, Fax: 042-255-6467, Email: daeyoung.yu@bng.or.kr
Received: September 6, 2019;  Revised: October 17, 2019;  Accepted: October 18, 2019.  Published online: October 31, 2019.
ABSTRACT
Objectives : This study was conducted to improve the analysis method used for acrylamide (AA) and to investigate the occurrence of AA in influent and effluent from sewage treatment plants in Korea. A liquid chromatography coupled to tandem mass spectrometry (LC–MS/MS) is commonly used for AA analysis of complex samples because it is fast, simple and effective. However, the disadvantages of LC–MS/MS include its relatively high operational cost, low sample throughput, and low sensitivity. Therefore, this study was conducted to develop a novel analytical method for the determination of AA in complex environmental waters using gas chromatography-mass spectrometry (GC/MS) combined with the derivatization with bromine following solid-phase extraction (SPE). Methods : This work describes the development of a novel SPE and GC/MS method for the analysis of AA in complex environmental waters. SPE parameters such as absorbent type, desorption solvent and volume were optimized by conducting a series of experiments. The best SPE cartridge was selected by conducting the recovery test with four different absorbents cartridge (SupelcleanTM Coconut Charcoal cartridge, SupelcleanTM ENVITM–Carb Tubes, Cleanert ODS C18 and Oasis HLB Cartridges). The brominated derivative, 2,3-dibromopropionamide (2,3-DBPA), was extracted with ethyl acetate (EA) and analyzed by GC/MS in selected ion monitoring (SIM), employing d3-acrylamide (d3-AA) as internal standard prior to extraction. Method validation was performed in terms of linearity of standard calibration curve, method detection limit (MDL), limit of quantification (LOQ), accuracy and precision of reaction product 2,3-DBPA.
Results
and Discussion : Based on the SPE experimental results, the active carbon SPE was selected as it gave the best adsorption efficiency (98.8%). The effects of pH and optimum bromine reaction time were found to be important determining factors for acrylamide analysis in water. The experimental results showed that the optimal reaction conditions of pH were 1.5 and 3 h, respectively. The validation process consisted of assessing the following parameters: linearity of standard calibration curve, method detection limit (MDL), limit of quantification (LOQ), precision and accuracy. The coefficients of determination (R2) in laboratory conditions were: R2=0.9981 (2.5~100 µg/L). MDL and LOQ of acrylamide were 1.19 µg/L and 3.79 µg/L, respectively. The recovery studies were carried out at two different concentration levels (10 µg/L and 50 µg/L, n=3). The intraday accuracy and precision were in the range of 100.6~102.0% and 3.2~3.5%, respectively, and the interday accuracy and precision were in the range of 96.0~97.4% and 4.3~8.0%, respectively. The AA contents in effluents of sewage treatment plants were in the range of 0.008~0.017 µg/L for May, 0.009~0.14 µg/L for June and not detected (N.D.)~0.02 µg/L for July samples.
Conclusions
: An efficient analytical method for the determination of AA has been developed. Activated carbon SPE cartridge (SupelcleanTM Coconut Charcoal) was selected for the sample purification. The validation study showed that this method was a reliable method with high sensitivity, linearity, precision, and accuracy. The interday accuracy and precision were in the range of 96.0~97.4% and 4.3~8.0%, respectively. This method was successfully applied to the determination of AA in effluent waters of sewage treatment plants. The AA contents in effluents of sewage treatment plants were in the range of 0.008~0.017 µg/L for May, 0.009~0.14 µg/L for June and not detected (N.D.)~0.02 µg/L for July samples.
Key Words: Acrylamide, Bromination, GC/MS, SPE
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