• 한국식품위생안전성학회지
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• 제18권2호
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• pp.43-50
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• 2003

A liquid chromatographic method, using matrix solid-phase dispersion (MSPD) is developed for the extraction of residual furazolidone in chicken eggs. Blank or fortified egg samples (0.5 g) were blended with Octadecylsilyl (Bulk $C_{18}$, 40${\mu}{\textrm}{m}$, 18%. load, endcapped. 2 g) derivatized silica. After homogenization, $C_{18}$/egg and Na$_2$S $O_4$matrix were transferred to a column made of 10 ml glass syringe and filter paper and compressed 4.0∼4.5 ml volume. The column was washed with 8 ml of hexane and dried under $N_2$ gas. Furazolidone was eluted with acetonitrile (8 ml) under gravity. The eluate containing furazolidone was free from interfering compounds when analyzed by HPLC with UV detection (365 nm, photodiode array). Calibration curves were linear (r = 0.99985) and inter- (1.47%) and intra-assay (5.29%) variabilities for the concentration range examined (7.8∼497 ng/g of eggs, 20 ${mu}ell$ injection volume) were indicative of an acceptable methodology for the analysis of furazolidone. Average recovery of furazolidone added to egg was 96.2%. The limit of detection for the proposed method was 1 ng/g for furazolidone. The method using MSPD is proposed as an alternative assay to the classical method which involves the use of large volumes of a harmful solvent and requires a long tedious separation and clean-up processes prior to its determination.

• Bulletin of the Korean Chemical Society
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• 제31권5호
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• pp.1143-1148
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• 2010

We investigated the separation of nitrogen heterocyclic compound (NHC) contained in a model coal tar fraction comprising four kinds of NHC [indole (In), quinoline (Q), iso-quinoline (iQ), quinaldine (Qu)], three kinds of bicyclic aromatic compound (BAC) [1-methylnaphthalene (1MN), 2-methylnaphthalene (2MN), dimethylnaphthalene (DMN) mixture with ten structural isomers (DMNs; regarded as one component)], biphenyl (Bp) and phenyl ether (Pe) by liquid membrane permeation (LMP). A batch-stirred tank was used as the permeation unit. An aqueous solution of saponin and n-hexane were used as the liquid membrane and the outer oil phase, respectively. Yield and selectivity of individual NHC was much larger than that of BAC, Bp and Pe. Increasing the initial mass fraction of the saponin to the membrane solution ($C_{sap,0}$) and the initial volume fraction of O/W emulsion to total liquid in a stirred tank (${\phi}_{OW,0}$) resulted in deteriorating the yield of individual NHC, but increasing the stirring speed (N) resulted in improving the yield of each NHC. With increasing $C_{sap,0}$, the selectivity of each NHC based on DMNs increased. Increasing ${\phi}_{OW,0}$ and N resulted in decreasing the selectivity of individual NHC based on DMNs. At an experimental condition fixed, the sequence of the yield and selectivity in reference to DMNs for each NHC was Q > Qu = iQ > In. Furthermore, we compared LPM method with methanol extraction method in view of the separation efficiency (yield, selectivity) of NHC.

• Korean Chemical Engineering Research
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• 제54권1호
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• pp.89-93
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• 2016

본 연구에서는 식물세포배양으로부터 항암물질 파클리탁셀 및 이의 반합성 전구체 10-디아세틸파클리탁셀의 분리 양상을 조사하였다. 식물세포인 바이오매스를 이용한 분리/정제 공정인 용매를 이용한 바이오매스 추출, 액-액 추출, 흡착제 처리, 헥산 침전, 분별 침전을 순차적으로 수행한 결과, 흡착제 처리 공정에서 10-디아세틸파클리탁셀는 파클리탁셀로부터 가장 효과적으로 분리됨을 알 수 있었다. 파클리탁셀 및 10-디아세틸파클리탁셀 분리에 적합한 흡착제 종류, 건조시료/흡착제 비율, 흡착제 처리 온도는 각각 실로퓨트, 1:1.5(w/w), $20^{\circ}C$ 이었다. 최적의 흡착제 처리 조건에서 10-디아세틸파클리탁셀은 74.1% 분리/회수 가능하였다.

• 분석과학
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• 제13권5호
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• pp.616-623
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• 2000

Phthalates 8종 및 adipate에 대해 수질 및 저질중의 함유량을 동시에 측정하였다. 수질의 경우는 n-헥산을 사용하여 액체-액체 추출법으로 추출하였고 농축시킨 후 n-헥산에 용해시켜서 분석하였으며 저질의 경우에는 디클로로메탄을 추출용매로 사용하여 초음파세정기를 이용하여 추출한 후 농축시켜서 이소옥탄에 용해시켜서 GC/MS에 주입하여 SIM 방법으로 분석하였다. 그 결과 0.1-20 ng/ml(수질)과 10-500 ng/g(저질, DEP: 10-250 ng/g; DEHP: 10-2000 ng/g)의 정량구간내에서 $R^2=0.993$ 이상의 좋은 직선성을 나타내었으며 검출한계는 0.1 ng/ml(수질)과 10 ng/g(저질) 이하이있다. 본 분석방법은 낮은 농도에서도 정밀도와 정확도가 양호하였다.

• 한국수산과학회지
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• 제42권1호
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• pp.15-19
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• 2009

A simple and sensitive method for erythromycin quantification by liquid chromatography electrospray mass spectrometry (LC-MS/MS) in fishery products was developed. Samples were extracted by liquid-liquid extraction using 70% acetonitrile. Lipids were removed by acetonitrile saturated hexane. LC separation was performed on a Shiseido UG C-18 column ($150\;mm{\times}2.0\;mm$ internal diameter.) with a gradient system of 0.2% acetic acid-acetonitrile containing 0.2% acetic acid as a mobile phase at flow rate of 0.2 mL/min. The mass spectrometer was operated in selected reaction monitoring with positive electro-spray interface. Transitions were monitored a m/z $734{\to}577$ and $734{\to}158$, with m/z $734{\to}577$ chosen for quantification. Recovery of erythromycin from fish and shrimp fortified at the 10 ng/mL, 50 ng/mL and 100 ng/mL were 91.6-109.4%, 84.4-111.2% and 98.8-109.6% with high precision, respectively. Limits of quantification and limits of detection of erythromycin in both fish and shrimp were 10.0 ng/mL and 1.0 ng/mL, respectively. This analysis method for erythromycin has been proposed for registration in the Korean Official Methods of Food Analysis and has been utilized for fishery products analysis by the Korea Food and Drug Adminstration and the National Fisheries Products Quality Inspection Service.

• Bulletin of the Korean Chemical Society
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• 제29권5호
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• pp.1043-1047
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• 2008

Simultaneous determination of amitraz, bromopropylate, coumaphos, cymiazole and 2,4-dimethylaniline in 200 honey samples purchased in Korea was performed by reversed-phase high-performance liquid chromatography with multiple UV detection. 2% Acetone in hexane was used for a liquid-liquid extraction and 20-40% water in acetonitrile solutions were used as mobile phases. The LOD for the analytes varied between 0.4 and 1.5 $\mu$g/L and the recoveries were yielded between 64 and 94%. Relative standard deviation of the repeatability of the method is less than 15%. Amitraz was not present in amount above 10 $\mu$ g/L and one for coumaphos and cymiazole and two for bromopropylate, and three for 2,4-dimethylanilne were detected in amount above 10 $\mu$ g/ L. Levels of the acaricide residues found were less than 50 $\mu$ g/L.

• 한국식품저장유통학회지
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• 제30권2호
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• pp.235-246
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• 2023

Yellowball (Citrus hybrid cv. Yellowball ) is a new citrus hybrid between Haruka (C. tamurana × natsudaidai ) and Kiyomi (C. unshiu × sinensis) and is known to possess strong antioxidant activity. However, detailed information on the antioxidant components of its peel has not yet been reported. This study evaluated the antioxidant activity of the peel and identified the antioxidant components by fractionating a methanolic extract of Yellowball peels using liquid-liquid extraction with n-hexane, ethyl ether (ether), ethyl acetate (EA), butanol, and water. The phenolic contents and antioxidant activities of the n-hexane, ether, and EA fractions were higher than those of the other fractions, and these fractions were further separated by semi-preparative high-performance liquid chromatography (HPLC). Four antioxidant peaks, EA1, EA2, EA3, and He1, were isolated and analyzed using ultra-performance liquid chromatography-quadrupole-time- of-flight mass spectrometry (UPLC-Q-TOF MS). Sinapoyl glucoside and hesperidin were identified in EA2 and EA3, respectively, and a polymethoxylated flavone (PMF) complex (5-hydroxy-3,6,7,8,3',4'-hexamethoxyflavone, natsudaidain, tetrameth- oxyflavone, and tangeretin) was identified in He1. A compound in EA1 with m/z 223.0246 [M-H] could not be identified and was named unknown2. The antioxidant activity of unknown2 (IC₅₀=69.17 ㎍/mL) was similar to that of Trolox, which was noted as a major antioxidant in Yellowball peel. Further studies on the antioxidant capacity of Yellowball peel are required; however, these results provide a foundation for using Yellowball peel as an antioxidant.

• 분석과학
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• 제19권3호
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• pp.244-254
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• 2006

난연제는 불길이 확산하거나 초기에 발생하는 것을 억제하는 물질을 의미한다. 난연제로 사용하는 이중 브롬계 난연제인 PBDEs는 갑상선 호르몬 붕괴와 내분비계 교란을 유발하는 물질이다. 본 연구에서는 PBDEs의 분석을 위한 적절한 전처리 방법을 제안하였고, 어류와 패류 포함 총 8종과 서울과 제주 모유 각 20개를 대상으로 BDE-28, 47, 99, 100, 153, 154 및 183의 인체 내 축적 수준을 조사하였다. PBDEs 분석을 위한 전처리 방법으로는 어패류의 경우 알칼리 분해 추출법을 적용하는 것이 적합한 것으로 확인되었다. 다층 실리카겔 컬럼 정제는 50 mL의 헥산을 이용하여 방해물질을 제거한후, 100 mL의 헥산:디클로로메탄(9:1)로 용출시키는 것이 적합한 것으로 확인되었다. 활성탄 정제 과정은 100 mL의 헥산:디클로로메탄(3:1)으로 용출시키는 것이 적합한 것으로 확인되었다. 어패류를 대상으로 한 실험에서 광어는 습식 중량 기준 890 pg/g이 검출되어, 시료 중 가장 높은 PBDEs 축적 정도를 보였다. 생태는 40 pg/g이 검출되어 시료 중 PBDEs의 축적 정도가 가장 낮은 것으로 나타났다. 모유 시료에서는 서울과 제주 지역에서 지방 중량 기준 2,580 및 3,600 pg/g이 검출되었으며, BDE-153과 183은 모두 검출되지 않았다. 재산과 초산의 경우 3,200 및 3,000 pg/g으로 큰 차이가 없는 것으로 나타났다. 본 연구에서 진행한 어패류 및 인체시료에서의 PBDEs 축적 정도를 파악한 결과, 외국에서 보고한 농도에 비해 낮은 수준을 유지하고 있음을 확인할 수 있었다.

• Bulletin of the Korean Chemical Society
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• 제24권5호
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• pp.559-565
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• 2003

An analytical method the determination of benzo(a)pyrene (BaP) and its hydroxylated metabolites, 1-hydroxybenzo(a)pyrene (1-OHBaP), 3-hydroxybenzo(a)pyrene (3-OHBaP), benzo(a)pyrene-4,5-dihydrodiol (4,5-diolBaP) and benzo(a)pyrene-7,8-dihydrodiol (7,8-diolBaP), in rat urine and plasma has been developed by HPLC/FLD and GC/MS. The derivatization with alkyl iodide was employed to improve the resolution and the detection of two mono hydroxylated metabolites, 1-OHBaP and 3-OHBaP, in LC and GC. BaP and its four metabolites in spiked urine were successfully separated by gradient elution on reverse phase ODS $C_{18}$ column (4.6 mm I.D., 100 mm length, particle size 5 ㎛) using a binary mixture of MeOH/H₂O (85/15, v/v) as mobile phase after ethylation at 90 ℃ for 10 min. The extraction recoveries of BaP and its metabolites in spiked samples with liquid-liquid extraction, which was better than solid phase extraction, were in the range of 90.3- 101.6% in n-hexane for urine and 95.7-106.3% in acetone for plasma, respectively. The calibration curves has shown good linearity with the correlation coefficients (R²) varying from 0.992 to 1.000 for urine and from 0.996 to 1.000 for plasma, respectively. The detection limits of all analytes were obtained in the range of 0.01-0.1 ng/mL for urine and 0.1-0.4 ng/mL for plasma, respectively. The metabolites of BaP were excreted as mono hydroxy and dihydrodiol forms after intraperitoneal injection of 20 mg/kg of BaP to rats. The total amounts of BaP and four metabolites excreted in dosed rat urine were 3.79 ng over the 0-96 hr period from adminstration and the excretional recovery was less than 0.065% of the injection amounts of BaP. The proposed method was successfully applied to the determination of BaP and its hydroxylated metabolites in rat urine and plasma for the pharmacokinetic studies.

• 분석과학
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• 제28권6호
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• pp.460-466
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• 2015

분유 내 콜레스테롤을 정량분석하기 위한 일차분석법으로 동위원소희석 질량분석법을 개발하였다. 내부표준물질로 콜레스테롤-d₄를 사용하여 분유에 첨가하였다. 분유에 지방산과 에스테르형태로 결합되어 있는 콜레스테롤을 자유 콜레스테롤로 바꾸어주기 위해 비누화과정을 수행하였다. 비누화과정은 반응온도, 반응시간, 사용한 KOH의 농도에 따라서 최적화하였으며, 그 결과로 분유시료 0.1 g에 대해 70 ℃에서 180 분 동안 8 M의 KOH 0.8 mL를 첨가하여 반응을 진행시키는 최적화조건을 확립하였다. 이와 같은 조건으로 실험을 진행하여 재현성은 0.23%, 확장불확도는 95%의 신뢰범위에서 1.9%로 추정되었다. 확립된 동위원소희석 질량분석법의 유효화를 위해 분유내에서 콜레스테롤의 인증값을 가지는 NIST SRM을 측정하였고 이 결과가 인증값과 불확도 범위내에서 일치하는 것을 확인하였다.