• 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.

• 한국식품위생안전성학회지
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• 제13권4호
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• pp.344-354
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• 1998

식육 및 우유 중에 고시된 설파제 등 16종 합성항균제를 HPLC로 동시에 정성, 정량할 수 있는 동시분석방법을 검토하였다. MSPD법으로 시료를 전처리를 하였으며 용출 용매로는 ethylacetat : acetonitrile(4:1)을 사용하였다. 이동사으로는 A 용매로 water : methanol : acetonitrile : phosphric acid(700: 250: 50: 0.2)와 B 용매로서 100% acetonitrile을 선택하여 그래디언트 컨트롤러를 사용하여 UV 266 nm에서 HPLC로 분석하였다. 현 식품공전법에 비해 유기용매는 99.1%, 실험단계는 94% 줄일 수 있어 분석시간과 인력은 95%, 비용은 98.8% 절감할 수 있었다. 각 시료의 평균 회수율은 닭고기에서는 67.7%, 96.2%, 소고기에서는 67.7%, 96.6% , 돼지고기에서는 70.0%, 96.2% 그리고 우유에서는 13.8%, 97.8%로 나타났다.

• 한국환경농학회지
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• 제28권3호
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• pp.266-273
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• 2009

HPLC를 이용한 분석은 항균, 항생제의 정량분석에 있어 가장 널리 이용되고 있으며, 최근에 개발된 MSPD방법은 고정상을 직접 갈아서 추출, 정제하는 방법으로 전처리 시 그조작이 간단하며, 유기용매가 적게 들고 전처리 시간이 짧다는 장점이 있다. 본 연구는 HPLC와 MSPD방법을 이용하여 가축 중 소비량이 가장 많은 돼지고기와 생선 중 회로 가장 많이 소비되는 광어에 대하여, 식품 중 잔류 가능성이 높은 tetracycline계 항생제 3종(oxytetracycline, tetracycline, chlortetracycline)과 sulfonamide(sulfadimethoxine, sulfamerazine, sulfamethazine, slfaquinoxaline, sulfamonomethoxine) 5종의 동시분석방법을 개발코자 하였다. HPLC의 최적 분석조건으로 파장은 tetracycline계 항생물질은 360 nm에서 sulfonamide는 270 nm였으며, 이동상은 TC와 SMR이 분리되는 시점인 15분까지는 pH 4.5, oxalic acid : acetonitrile (78.5 : 21.5, v/v)로 분석하고 이후 30분까지는 pH 6.1, oxalic acid : acetonitrile (78.5 : 21.5, v/v)로 분석을 실시하였을 때 기존의 실험방법보다 피크의 분리도와 검출한계의 개선이 이루어졌으며 이를 토대로 8가지 성분의 MRLs인 $0.1{\sim}0.2mg{\cdot}kg^{-1}$까지 충분히 분석이 가능하였다. MSPD 적용을 위한 시료의 전처리 방법개선은 기존의 0.5 g으로 제한된 시료량을 3 g으로 늘릴 수 있었고 dichloromethane 20 mL와 methanol 20 mL로 연속적으로 8가지 성분을 동시에 용출시켜 sulfonamide는 $80.25{\sim}101.25%$, tetracycline계 항생물질은 $85.77{\sim}121.42%$의 회수율을 얻을 수 있었다.

• 한국동물위생학회지
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• 제26권3호
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• pp.199-202
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• 2003

Solid phase extraction(SPE) and matrix solid phase dispersion(MSPD) have been studied as preparation procedures for tetracyclines analysis by high-performance liquid chromatography(HPLC) in meat. The recovery range was 74${\sim}$98% for SPE, and 72${\sim}$93% for MSPD at spiked levels of 100ng/g for oxytetracycline(OTC), tetracycline(TC), chlortetracycline(CTC), and doxycycline(DC). The detection limits were 15${\sim}$78ng/g for SPE and 25${\sim}$84ng/g for MSPD, respectively. Analytical method was HPLC with UV detector. The purpose of this study was developing a practical, accurate and precise method for rapid extraction and quantitation of tetracycline residues in meat.

• 한국동물위생학회지
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• 제22권1호
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• pp.15-23
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• 1999

A multiresidue, simple and rapid isolation technique known as matrix-solid phase dispersoin (MSPD) for the extraction and quantitative gas chromatographic/electron capture detection (GC/ECD) determination of 14 organochlorinated pesticides($\alpha$-BHC, ($\beta$-BHC, ($\gamma$-BHC, aldrin, dieldrin, endrin, heptachlor, ($\alpha$-endosulfan, ($\beta$-endosulfan, endosulfan sulfate, p,p'-DDE, o,p'-DDD, p,p'-DDD, p,p'-DDT) from meat fats. The 14 pesticide were fortified into meat fat(0.5g) and blend with 2g $C_{18}$, $C_{18}$meat fat matrix blend and 2g activated florisil comprise an extraction column from which the pesticides are eluted by adding 8ml acetonitrile. Then 2${\mu}\ell$ of the eluate is analyzed by GC/ECD. Unfortified blank controls are tested similarly. The eluate contained all the pesticide analytes and was free of interfering coextractants. Recovery rate(31.3-500ng/g) were ranged from 80$\pm$4% to 97$\pm$4%. Any organochlorinated pesticides were not detected in 120 samples of beef and pork collected from slaughter houses in Kyeonggi province.

• 한국동물위생학회지
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• 제19권2호
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• pp.163-171
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• 1996

This study was carried out to determination of carbadox and olaquindox residues in swine tissues by MSPD(matrix solid phase disperse)method. The results obtained were as follows ; 1. Optimal wavelengths of UV for carbadox and olaquindox were 310 and 370nm, respectively 2. Ethyl acetate-Acetonitrile(8:2) was found to be adequate as extractant in this method. 3. The average overall recovery of carbadox at the 0.01, 0.05, and 1.0PPM spike levels was 89. 2% and that of olaquindox was 89.9%, and the detection limits were 0.5ng for carbadox and olaquindox.

• 한국식품위생안전성학회지
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• 제12권2호
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• pp.117-124
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• 1997

A simple, rapid and simultaneous analytical method is described for the detection of Sulfonamide and Tetracycline residues, i.e., Sulfamerazine (SMR), Sulfamethazine (SMT), Sulfamonomethoxine (SMM), Sulfadimethoxine (SDM), Sulfaquinoxaline (SQN), Oxytetracycline (OXY), Tetracycline (TC), Chlortetracycline (CTC). Blank control and sulfonamide and tetracycline fortified fish muscle samples (0.5 f) were blended with octadecylsilyl (C18, 40 ${\mu}{\textrm}{m}$, 21% load, 60$\AA$) derivatized silica packing material (2 g). Blended fish samples were washed with hexane, then, benzene and dichloromethace were used for the elution of tetracycline and sulfonamide were analyzed by HPLC. Correlation coefficients of standard curves for individual sulfonamide and tetracycline isolated from fortified samples were linear (0.9993$\pm$0.0003~0.9997$\pm$0.0003, 0.9493$\pm$0.078~0.9753$\pm$0.036), respectively. The average percentage recoveries of sulfonamide and tetracycline ranged as 80.86~96.52% to 85.88~92.23%, and 30.01~37.12% to 65.89~73.40%, for the concentration range (0.1~1.0 ppm) examined, respectively. Limit of detection for sulfonamide was 0.0012 ppm for SMR in Paralichthys Olivacleus and 0.0020 ppm for SMR, 0.015 ppm for SMM in Cyprinus Carpio. The applicability of this procedure is demonstrated by separation and detection of incurred tetracycline and sulfonamide residues in fish muscle tissue.

• 한국연초학회지
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• 제36권1호
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• pp.12-19
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• 2014

A matrix solid-phase dispersion (MSPD) method was developed for extracting and cleaning-up the selected agrochemicals in tobacco using gas chromatography-mass spectrometry with selected ion monitoring (GC/MS-SIM). Different parameters of the method were investigated and optimized, such as the type of solid-phase (alumina, $C_{18}$ and Florisil) and eluent (acetone, acetonitrile, ethylacetate and n-hexane). The best results were obtained using 0.5 g of tobacco sample, 1.0 g of $C_{18}$ as dispersant sorbent, 1.0 g of Florisil as clean-up sorbent and acetonitile saturated with n-hexane as eluting solvent. The method was validated using tobacco samples fortified with agrochemicals at their different concentration levels. This method gave good linearity for the selected agrochemicals of ranging from $0.01{\mu}g/mL$ to $0.1{\mu}g/mL$. Recoveries of the selected agrochemicals in tobacco were more than 80 % and reproducibilities were found to be better than 10 % RSD. Those results suggested that the analytical procedure including MSPD method in combining with GC/MS could be applicable to the rapid determination often the selected agrochemicals in tobacco.

• 농약과학회지
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• 제4권1호
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• pp.26-31
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• 2000

콩나물중 잔류농약의 효율적인 분석법을 확립하기 위하여 carbendazim과 thiabendazole을 0.1, 0.3, 0.5 mg/kg 씩 첨가하여 농약성분의 추출방법을 비교하였고, 잔류성을 평가하기 위하여 thiophanate-methyl 1.0, 2.0 g/L 용액에 수침시킨 콩으로 콩나물을 재배하면서 매일 잔류량을 조사하였으며, 또한 시중에 유통되는 콩나물중 benzimidazole계 농약의 잔류실태 조사를 실시하였다. 추출방법에 따라 carbendazim의 회수율은 LLE $69.25{\sim}79.16%$, SPE $79.99{\sim}90.42%$, MSPD $92.40{\sim}98.48%$이었으며, thiabendazole의 회수율은 LLE $64.86{\sim}83.26%$, SPE $79.12{\sim}94.04%$, MSPD $65.44{\sim}73.92%$로 고체상 추출방법이 우수하였다. 또 재배기간별 carbendazim 잔류량은 콩나물 출하적기인 재배 5일 째 $0.10{\sim}0.25$ mg/kg이었으며, 출하적기를 넘긴 7일째에도 농약이 잔류되었다. 유통 콩나물 448건을 검사한 결과 6건에서 carbendazim이 검출되었고 검출량은 3건에서 0.1 mg/kg 미만이었으나 3건에서는 0.1 mg/kg을 초과하여 최대 0.37 mg/kg까지 검출되었다.

• 한국가축위생학회:학술대회논문집
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• 한국가축위생학회 1999년도 제22차 학술대회
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• pp.188.2-189
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• 1999