• Journal of Food Hygiene and Safety
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• v.18 no.2
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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.

• Journal of Food Hygiene and Safety
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• v.13 no.4
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• pp.344-354
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• 1998

This study was conducted to evaluate the MSPD and HPLC method about simultaneous determination for residual synthetic antimicrobials of sixteen species such as sulfonamide etc. in livestock products. Elution solvent used in HPLC was ethylacetate:acetonitrile (4:1), and mobile phases for solvent A and B were water:methanol:acetonit rile:phosphric acid (700:250:50:0.2) and 100% acetonitrile respectively. The detector and absorbency used in HPLC was UV 266 nm. This study showed the reduction effect of 99.1% for organic solvents, 94% for experimental steps, 95% for analytical time and manpower and 98.9% for costs compared with korea food standard method. The average recovery rates for chicken, bovine, pork and milk were 67.7% 96.2%, 67.7%~96.6%, 70.0%~96.2%, and 13.8%~97.8%.

• Korean Journal of Environmental Agriculture
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• v.28 no.3
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• pp.266-273
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• 2009

This study was conducted to develop more convenient simultaneous determination method by matrix solid phase dispersion (MSPD) and HPLC for sulfonamides such as sulfamerazine (SMR), sulfamethazine (SMT), sulfamonomethoxine (SMM), sulfadimethoxine (SDM), sulfaquinoxaline (SQX), and tetracyclines including oxytetracycline (OTC), tetracycline (TC) chlortetracycline (CTC) in prok and flatfish. The limits of detection were 0.047 $mg{\cdot}kg^{-1}$ for OTC, TC, SMR, SMT and SMM, and 0.033 $mg{\cdot}kg^{-1}$ for CTC, SDM, and SQX, respectively. So it is sufficiently possible to detect the eight tetracyclines and sulfonamides under their MRLs ($0.1{\sim}0.2mg{\cdot}kg^{-1}$). The average percentage recoveries of sulfonamides and tetracyclines from pig muscle and flatfish spiked standard solution were approximately $80.25{\sim}101.25%$ and $85.77{\sim}121.42%$, respectively. Therefore this method was efficient for simultaneous analysis of eight tetracyclines and sulfonamides.

• Korean Journal of Veterinary Service
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• v.26 no.3
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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.

• Korean Journal of Veterinary Service
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• v.22 no.1
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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.

• Korean Journal of Veterinary Service
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• v.19 no.2
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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.

• Journal of Food Hygiene and Safety
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• v.12 no.2
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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.

• Journal of the Korean Society of Tobacco Science
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• v.36 no.1
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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.

• The Korean Journal of Pesticide Science
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• v.4 no.1
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• pp.26-31
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• 2000

An analytical method was approached to determine the residues of benzimidazole fungicides in soybean sprouts and was compared with traditional solvent-based method of extraction, solid phase extraction(SPE) and matrix solid phase dispersion(MSPD). The recoveries of carbendazim for liquid-liquid extraction (LLE), SPE and MSPD in soybean sprouts were $69.25{\sim}79.16$, $79.99{\sim}90.42$ and $92.40{\sim}98.48%$, respectively. The recoveries of thiabendazole for LLE, SPE and MSPD in soybean sprouts were $64.86{\sim}83.26$, $79.12{\sim}94.04$ and $65.44{\sim}73.92%$, respectively. The residues of carbendazim by elapsed time under our cultivated soybean sprouts program found $0.10{\sim}0.25$ mg/kg after 5 days and trace concentration of carbendazim was detected after 7 days. Of the 448 samples analyzed, less than 1.5% had residues of carbendazim ranged from 0.05 to 0.37 mg/kg.

• Proceedings of the Korean Society of Veterinary Service Conference
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• 1999.05a
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• pp.188.2-189
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• 1999