• Journal of Food Hygiene and Safety
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• v.8 no.3
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• pp.147-150
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• 1993

A novel rapid and sensitive method to detennine residual oxolinic acid in Acetes japonicus was developed. The residual oxolinic acid was extracted with ethylacetate and diluted oxalic acid, and interfering substances were removed by hexane. Fifty ppb residual concentration in the extract could be quantitated by UV-HPLC and the recovery rates were 79-91% according to the fortified amounts.

• Journal of Food Hygiene and Safety
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• v.37 no.3
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• pp.143-148
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• 2022

This study was to investigate an analytical method for determining dieckol content in Ecklonia stolonifera extract. According to the guidelines of International Conference on Harmonization. Method validation was performed by measuring the specificity, linearity, precision, accuracy, limit of detection (LOD), and limit of quantification (LOQ) of dieckol using high-performance liquid chromatography-photodiode array. The results showed that the correlation coefficient of calibration curve (R²) for dieckol was 0.9997. The LOD and LOQ for dieckol were 0.18 and 0.56 ㎍/mL, respectively. The intra- and inter-day precision values of dieckol were approximately 1.58-4.39% and 1.37-4.64%, respectively. Moreover, intra- and inter-day accuracies of dieckol were approximately 96.91-102.33% and 98.41-105.71%, respectively. Thus, we successfully validated the analytical method for estimating dieckol content in E. stolonifera extract.

• Proceedings of the Korean Environmental Sciences Society Conference
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• 2008.11a
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• pp.248-251
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• 2008

일반적으로 phthalate esters의 전처리방법에는 액액추출법(liquid-liquid extraction), 고상추출법(Solid-phase Extraction, SPE), 고상미세추출법(Solid-phase micro extraction, SPME) 등의 분석방법이 있다. 그 중에서 본 연구에서는 SPE를 이용하여 간편하고 정확성이 높으며, 적은 양의 유기용제를 사용하여 전처리함으로써 2차적인 환경오염을 줄일 수 있다는 점에서 다른 전처리 방법보다 유용하다고 할 수 있다. 검출감도 측면에서 phthalate esters의 경우는 구조적으로 안정적인 편이나 페놀류의 경우 hydroxy group 때문에 GC/MS 분석시 유도체화 과정이 필수적인데 이번 연구에서 사용한 BSTFA/TMCS는 비교적 쉽고 빠르게 유도체 화할 수 있다는 이점이 있다. 더 많은 연구가 필요하겠지만 앞서서의 결과에서도 알 수 있듯이 전반적으로 검출한계가 0.05$\sim$0.5 $\mu$g/L 정도로 높고, 4-nonyl phenol을 제외하고 80% 이상의 양호한 회수율을 나타낸 것으로 미루어 보아 phthalate esters, phenols의 효율적인 동시분석이 가능함을 알 수 있다.

• Analytical Science and Technology
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• v.15 no.3
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• pp.300-316
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• 2002

The extraction methods of PBBs from environmental samples by soxhlet extraction for solid phase and liquid-liquid extraction for liquid phase were compared. After extraction, silicagel and florisil as column clean up methods were used for the comparison of cleanup efficiency with different solvent system. Also, the analytical instruments were used GC/MSD. The 22 kinds of PBBs standards were used to establish the analytical methods to perform the experiments of recoveries and detection limits in water and soil. The detection limits of PBBs represented 5~10 ng/L for water and 0.5~3.5 ng/g for soil samples, respectively. The recoveries of water samples represented 96~107% in n-hexane, dichloromethane and toluene for water, and 60~80% in combined solvent with n-hexane and acetone. The recoveries of soil sample were surveyed 67~97% in soxhlet extraction and 64~76% in ultrasonic extraction with selected solvents.

• Journal of Korean Society of Environmental Engineers
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• v.31 no.1
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• pp.64-69
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• 2009

Musty and earth odors caused by geosmin and 2-MIB are the major complaints from the drinking water consumers. Therefore, early detection of geosmin and 2-MIB is the key to prevent off-flavor occurrence. In this study, a rapid method using stir bar sorptive extraction (SBSE) in combination with the GC/MS was investigated to analyze geosmin and 2-MIB in water. The SBSE method, a solventless extraction technique, was optimized and then applied to the analysis of geosmin and 2-MIB in water. The SBSE technique was found to be a simple and fast procedure that allows many samples to be extracted simultaneously using very small volume (10~20 mL). In addition, the SBSE method offered high recovery and good linear regression coefficient for the geosmin and 2-MIB. The good repeatability of this method can be deduced from the low RSD (7.2~7.6%) at 10 ng/L for geosmin and 2-MIB. The limit of detection was determined 1~2 ng/L and the limit of quantitation was 3~6 ng/L. Above all, the SBSE method proved to be a very practical technique for the analysis of geosmin and 2-MIB in water.

• Journal of Food Hygiene and Safety
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• v.39 no.2
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• pp.152-162
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• 2024

In this study, we investigated the levels of the natural preservatives, benzoic acid, sorbic acid, and propionic acid, in raw unprocessed vegetables. Quantitative analysis of benzoic acid and sorbic acid was performed using high-performance liquid chromatography with a diode array detector (HPLC-DAD) and confirmed using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Propionic acid was analyzed using a gas chromatography-flame ionization detector (GC-FID) and confirmed using gas chromatography-mass spectrometry (GC-MS). From a total of 497 samples, benzoic acid, sorbic acid, and propionic acid were found in 50 (10%), 8 (0.2%), and 61 samples (12.3%), respectively. The highest quantity of benzoic acid, sorbic acid, and propionic acid was found in peony root (1,057 mg/kg), nut-bearing torreya seeds (27.3 mg/kg), and myrrha (175 mg/kg), respectively. The background concentration range of naturally occurring preservatives in raw vegetables determined in this study could be used as standard inspection criteria to address consumer complaints and trade disputes.

• Analytical Science and Technology
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• v.15 no.3
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• pp.196-213
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• 2002

The alkylphenols, chlorophenols and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring mode followed by three work-up methods for comparison; EPA method, isoBOC derivatization method and TBDMS derivatization method. Eleven phenols in water samples were extracted with dichloromethane. Also, solid-phase extraction (SPE) with XAD-4 and subsequent conversion to isobutoxycarbonyl derivatives or tert.-butyldimethylsilyl derivatives for sensitive analysis with the selected ion-monitoring (SIM) mode. The recoveries were 85.1~109.9% (EPA method) and 90.3~126.6% (isoBOC derivatization and TBDMS derivatization), respectively. The method detection limit of bisphenol A for SIM were 0.732 ${\mu}g/{\ell}$ (EPA method), 0.002 ${\mu}g/{\ell}$ (isoBOC derivatization) and 0.021 ${\mu}g/{\ell}$ (TBDMS derivatization). The SIM responses were linear with the correlation coefficient varying 0.9755~0.9981 (isoBOC derivatization), and 0.9908~0.9996 (TBDMS derivatization). When these methods were applied to treated wastewater sample from a polyethylene plant, the concentrations of 11 phenols were below the method detection limit.

• The Journal of Korean Institute of Communications and Information Sciences
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• v.16 no.12
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• pp.1229-1235
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• 1991

본 연구에서는 음향파의 입사각을 횡파임계각도 이상으로 하여 횡파를 발생시키고 이를 이용하여 종래방식보다 고체 내부에 존재하는 미소결함의 검출한계를 개선시키는 방법을 연구분석하였다. 실험을 위하여 중심주파수3MHz인 반사형 음향현미경 시스템을 구성하였고 서로 다른 깊이에 임의의 결함을 갖는 시료를 제작하였으며 defocus 깊이를 변화시키면서 실험하였다. 실험결과 고체내부 Rayleigh파장의 3배정도 깊이에 존재하는 1mm 크기의 결함을 검출할 수 있었다.

• Journal of the Korean Society of Food Science and Nutrition
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• v.46 no.9
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• pp.1091-1096
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• 2017

The aim of this study was the validation of a modified analytical method for determination of oxypaeoniflorin and paeoniflorin in Moutan Cortex Radicis extract. For validation of the analytical method, we modified established analytical methods and validated improvement. For validation, the specificity, linearity, precision, accuracy, limit of detection (LOD), and limit of quantification of oxypaeoniflorin and paeoniflorin were measured by high performance liquid chromatography. The results show that the correlation coefficients of the calibration curve for oxypaeoniflorin and paeoniflorin were 1.0000 and 0.9998, respectively. The LOD for oxypaeoniflorin and paeoniflorin were $0.23{\mu}g/mL$ and $0.25{\mu}g/mL$, respectively. The inter-day and intra-day precision values of oxypaeoniflorin and paeoniflorin were 0.70~3.19% and 1.74~2.43%, and 0.32~0.92% and 0.62~2.28%, respectively. The inter-day and intra-day accuracies of oxypaeoniflorin and paeoniflorin were 98.33~102.11% and 97.72~118.12%, and 98.44~101.56% and 97.10~112.00%, respectively. Therefore, the analytical method was validated for the detection of oxypaeoniflorin and paeoniflorin in Moutan Cortex Radicis.

• Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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• 2005.04a
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• pp.31-35
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• 2005

본 연구는 토양에 휘발유 첨가제인 MTBE와 휘발유의 주성분인 BTEX를 headspace 법에 의해 동시 분석하는 방법이다. 인산으로 pH를 2로 조절한 후 NaCl로 포화시킨 용액 5ml를 헤드스페이스 바이알에 보존제로 넣은 후 토양시료 약 2g을 이 용액에 침지시켜 시료 채취한 다음 헤드스페이스 장치에 넣고 $80^{\circ}C$에서 40분 가온하여 상부 기상의 일정량을 취해 GC-MS (SIM)으로 분석하였다. 본 분석법에 의한 검출한계는 methyl-tert-butyl ether(MTBE)와 benzene, toluene, ethylbenzene, o,m,p-xylene(BTEX)이 각각 0.1, 0.1, 0.1, 0.2, 0.1, 0.2 ng/g이었고, 직선성은 0.995이상이었으며, 재현성도 10%내외의 정밀한 값을 보였다. 실제 시료를 분석한 결과, MTBE가 3-6,993 ng/g의 농도분포를 보였고 total BTEX는 1 ng/g으로 검출되었다. 이 방법은 빠르고 정밀 정확한 분석법으로 공정시험법으로 활용가치가 높다.