GC-MS를 이용한 하천수 중 Bisphenol계 화합물의 동시분석 및 모니터링
Simultaneous Determination and Monitoring of Bisphenols in River Water using Gas Chromatography-Mass Spectrometry
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본 연구는 하천수 중 bisphenol계 화합물 6종(BPA, BPB, BPC, BPE, BPF, BPS)을 동시분석하기 위하여GC-MS를 이용하였다. 또한 최적의 전처리 방법을 확립하고자SPE 및 LLE법을 이용하여 표준시료로부터 검량선의 직선성, MDL, LOQ, 정확도 및 정밀도를 비교하였다. SPE 및 LLE 전처리 방법에 의한 MDL은 각각 0.0005∼0.0234 μg/L와0.0037∼0.2034 μg/L, LOQ는 각각 0.0015∼0.0744 μg/L 와 0.0117∼0.6477 μg/L, 검량선의 결정계수(r2)는 모두0.9969 이상, 정확도는 각각 93.2∼108%와 97.4∼120%, 정밀도는 각각 1.7∼4.6%와 0.7∼6.5% 범위로 만족한 정도관리 결과를 얻었다. 하지만 SPE법에 의한 MDL 및 LOQ 값은 LLE법보다 약 4∼45배 정도 높은 감도를 보였고, 특히BPA의 경우는 다른 화합물들보다 45배 정도 높았다. 따라서, 본 연구에서는 SPE법을 적용하여 하천수 시료를 분석하였고, 조사지점은 본류 7개, 지류 6개, 하수종말처리장 2개 지점을선정하였다. Bisphenol계 화합물 중에서 BPB, BPC, BPE, BPF 및 BPS는 모두 불검출 되었으나, BPA 농도는 0.0095 ∼0.2583 μg/L 범위로 본류 0.0166∼0.0810 μg/L, 지류0.0095∼0.2583 μg/L, 하수종말처리장 0.0352∼0.1217 μ g/L으로 미량 수준이었다.
Abstract
BACKGROUND:This studywas carried out to establish an efficient sample preparation for the simultaneous determination of bisphenols (BPs) in river water samples using gas chromatography-mass spectrometry (GC-MS). Sample preparation was examined with conventional extraction methods, such as solid-phase extraction (SPE) and liquid-liquid extraction (LLE), and their efficiencywas compared with validation results, including linearity of calibration curve, method detection limit (MDL), limit of quantification (LOQ), accuracy, and precision. METHODSANDRESULTS:TheBPs (bisphenolA, BPA; bisphenol B, BPB; bisphenol C, BPC; bisphenol E, BPE; bisphenol F, BPF; bisphenol S, BPS) were analyzed using GC-MS. The range ofMDLs by SPE and LLEmethodswas 0.0005∼0.0234 μg/L and 0.0037∼0.2034 μg/L, and that of LOQswas 0.0015∼0.0744 μg/L and 0.0117∼0.6477 μ g/L, respectively. The calibration curve obtained from standard solution of 0.004∼4.0 μg/L(SPE) and 0.016∼16 μg/L (LLE) showed good linearity with r2 value of 0.9969 over. Accuracy was 93.2∼108% and 97.4∼120%, and precisionwas 1.7∼4.6%and 0.7∼6.5%, respectively. The values of MDL and LOQ resulted from the SPE method were higher than those from the LLE method, particularly those values of BPAwere highest among theBPs. Based on the results, the SPE method was applied to determine the BPs in river water samples. Water samples were collected from mainstream, tributary and sewage wastewater treatment plants (SWTPs) in theYeongsan river basin. The concentration of BPB, BPC, BPE, BPF andBPSwere not detected in all sites, whereas BPA was ranged 0.0095∼ 0.2583 μg/L, which was 0.0166∼0.0810 μg/L for mainstreams, 0.0095∼0.2583 μg/L for tributaries, 0.0352 ∼0.1217 μg/L for SWTPs. CONCLUSION: From these results, the SPE method was very effective for the simultaneous determination of BPs in river water samples using GC-MS.We provided that it is a convenient, reliable and sensitive method enough to monitor and understand the fate of the BPs in aquatic ecosystems.
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