• Title, Summary, Keyword: MSPD

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Analysis of synthetic Antimicrobials in Livestock Products by MSPD Method (MSPD법에 의한 축산물 중 합성항균제 동시분석)

  • 김재관;도영숙;박준조;황혜정
    • 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%.

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Simultaneous Determination of Tetracyclines and Sulfonamides Residues in Pork and Flatfish Using Matrix Solid Phase Dispersion (MSPD) Extraction and HPLC (MSPD와 HPLC를 이용한 돼지고기 및 광어 중의 테트라싸이클린계 항생제와 sulfonamide의 다성분 잔류분석법 개발)

  • Gil, Geun-Hwan;Ko, Kwang-Yong;Lee, Yong-Jae;Park, Hye-Jin;Lee, Kyu-Seung
    • 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.

Screening procedure for organochlorinated pesticide residues in meat fat using a matrix solid phase dispersion(MSPD) extraction and GC/ECD (MSPD법과 GC/ECD를 이용한 식육중의 잔류농약 분석)

  • 백미순;이영철;박병옥;김창수;박유순
    • 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.

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Comparison of pretreatment methods for tetracyclines analysis by HPLC (테트라싸이클린계 잔류항생물질 분석을 위한 전처리방법 비교)

  • Kim, Dong-Eon;Hwang, Lae-Hwong;Yun, En-Sun;Ham, Hee-Jin;Yang, Yoon-Mo;Kim, Chang-Gi;Ki, No-Jun;Lee, Jung-Hark
    • 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.

Matrix Solid-Phase Dispersion (MSPD) Isolation and Liquid Chromatographic Determination of Residual Furazolidone in Eggs (MSPD 전처리법과 HPLC를 이용한 Furazolidone의 계란내 잔류분석)

  • 서계원;이재일;이채용;이정치
    • 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.

A study on determination of carbadox and olaquindox in swine tissues by matrix solid Phase disperse method" (MSPD 방법에 의한 돈육중 Carbadox와 Olaquindox 분석법 연구)

  • 황래홍;김영수;김기근
    • 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.

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Simultaneous Quantification of Sulfonamide and Tetracyclines in Fish Muscle Tissue by Matrix Solid Phase Dispersion (MSPD) Extraction and HPLC (MSPD와 HPLC를 이용한 어류의 잔류 설파제와 테트라사이클린계 항생물질의 동시분석)

  • 하대식;김종수;김곤섭
    • 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.

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Determination of agrochemical residues in tobacco using matrix solid-phase dispersion and GC/MS

  • Lee, Jeong-Min;Min, Hye-Jeong;Park, Jin-Won;Lee, Moon-Young;Jang, Gi-Chul
    • 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.

An extraction method and residues of benzimidazole fungicides in soybean sprouts (콩나물중 benzimidazole계 농약의 추출방법과 잔류성)

  • Park, Jun-Jo;Yong, Kum-Chan;Jeung, Jin-A
    • 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.

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A assessment of multiscale-based peak detection algorithm using MIT/BIH Arrhythmia Database (MIT/BIH 부정맥 데이터베이스를 이용한 다중스케일 기반 피크검출 알고리즘의 검증)

  • Park, Hee-Jung;Lee, Young-Jae;Lee, Jae-Ho;Lim, Min-Gyu;Kim, Kyung-Nam;Kang, Seung-Jin;Lee, Jeong-Whan
    • The Transactions of The Korean Institute of Electrical Engineers
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    • v.63 no.10
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    • pp.1441-1447
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    • 2014
  • A robust new algorithm for R wave detection named for Multiscale-based Peak Detection(MSPD) is assessed in this paper using MIT/BIH Arrhythmia Database. MSPD algorithm is based on a matrix composed of local maximum and find R peaks using result of standard deviation in the matrix. Furthermore, By reducing needless procedure of proposed algorithm, improve algorithm ability to detect R peak efficiently. And algorithm performance is assessed according to detection rates about various arrhythmia database.