• 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.

• Korean Journal of Veterinary Service
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• v.27 no.1
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• pp.17-29
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• 2004

A multiresidual analysis was performed to determine 12 sulfonamides(sulfacetamide, sulfadiazine, sulfisomidine, sulfathiazole, sulfapyridine, sulfamerazine, sulfamethazine, sulfamonomethoxine, sulfisoxazole, sulfamethoxazole, sulfaquinoxaline, and sulfadimethoxine) in beef and pork simultaneously. The multiresidual analysis for the sulfonamides currently used was able to analyze 5 kinds of sulfonamides at the same time. The method of this 12 sulfonamides multiresidual analysis in this study was matrix solid-phase dispersion(MSPD) by high performance liquid chromatography (HPLC) and liquid chromatography mass spectrometry (LC/MS). The recovery rate of the materials was measured by MSPD method with 3 different extraction solvents; Dichloromethane, DCM: Ethylacetate(3:1), DCM:EA(9:1). Also, samples (84 beef and 205 pork samples) which were positive by EEC-4 plate test from 2001 to 2003 were tested to investigate the kinds of sulfonamides using HPLC. The results from the study were as follows; 1. The recovery rate of the materials was measured by MSPD method with 3 different extraction solvents; Dichloromethane, DCM:Ethylacetate(3:1), DCM:EA(9:1). The method of extraction solvent with DCM:ethyl acetate(9:1) was the most excellent(87.7∼99.3%) in separation and reappearance. 2. In the LC/MS analysis. of sulfonamides, signal to noise ratio was showed relatively high in the positive mode and special ion in the quality analysis was determined via [M+H]$\^$+/ and m/z 156. A spectrum of sulfonamides was showed from all 12 sulfonamides. 3. The samples positive by the EEC-4 plate, a screening test method, were categorized by sulfonamides through Charm II and confirmed the kinds of sulfonamides through HPLC. 1) Among 84 beef samples positive by EEC-4 plate, 20 samples were positive by Charm II and identified as 7 sulfamethazine, 9 sulfadimethoxine, 1 sulfamonomethoxine and 3 unknown status. 2) Among 205 pork samples positive by EEC-4 plate, 42 samples were positive by Charm II and identified as 19 sulfamethazine, 1 sulfadimethoxine, 4 sulfamonomethoxine and 5 unknown status.

• Korean Journal of Veterinary Service
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• v.29 no.3
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• pp.317-330
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• 2006

This study was conducted to develop the analytical method about simultaneous determination for synthetic antimicrobials in muscle by high performance liquid chromatography - mass selective detector (HPLC- MSD). Solid phase extraction (SPE), matrix solid phase dispersion (MSPD) and liquid-liquid extraction (LLE) have been adapted as pretreatment procedures for HPLC- MSD. Among various solvent tested, methanol was chosen for extraction of synthetic antimicrobials in muscles. For the optimized response, the values of various MS parameters including fragment voltage, drying gas flow, nebulizer pressure, drying gas temperature were verified. The average recovery rates using MSPD and SPE for muscles of bovine and pork were 78.9-127.1% and 78.3-121.7%, respectively. This method was verified the satisfactory performance for fourteen synthetic antimicrobials excepting carbadox in muscle of pork as detection limit of $0.05{\mu}g/g$ on API/ES SIM mode.

• Korean Journal of Veterinary Service
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• v.18 no.3
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• pp.13-28
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• 1995

This study was carried out to explore the most sensitive and useful method for simultaneous determination of five sulfa drugs(sulfamethazine, sulfamerazine, sulfamonomethoxine, sulfadimethoxine, sulfaquinoxaline) in livestock productions(pork muscle, bovine muscle, chicken muscle, milk ) by HPLC with UV detector and reverse phase column. The results obtained were as follows：1. For mobile phase acetonitrile-0.01M ammonium acetate (23：77) showed more applicable sensitivity and retention times than acetonitrile-1% acetic acid(23：77). Thus acetonitrile-0.01M ammonium acetate(23：77) selected and applied to the modification test, from which it was found pH 6.75 was the most adequate. 2. Optimal wavelength of UV for SMT(sulfamethazine), SMR(sulfamerazine), SMM(sulfamonomethoxine), SD(sulfadimethoxine), and SQ(sulfaquinoxaline) were 266, 266, 265, 269 and 250nm, respectively, and that for simultaneous application it was 263nm. 3. The average recovery rate by extractant(chloroform, dichloromethane, chlorform+dich-loromethane) in the classic method was not significantly different(p>0.05) but that by chloroform higher than the others. Thus chloroform was found to be adequate as extractant in this classic method. 4. The average recovery rate was 86.5% by the MSPD(matrix solid phase disperse) method, which was significantly higher than that by the classic method(p<0.05). Also the recovery rates by method were significantly different(p<0.05) in accordance with sample and type of drug. The MSPD method was much superior to classic method on clean-up.

• Korean Journal of Veterinary Service
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• v.26 no.2
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• pp.145-149
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• 2003

To explore the most sensitive and useful method for simultaneous determination of 8 carbamate pesticides in livestock productions, the mixture of 8 carbonates was determined by HPLC with scanning fluorescence detector. For mobile phase water, acetonitrile and methanol program gradient showed more applicable sensitivity than water and acetonitrile program gradient used ExW 339 nm and EmW 445 nm for fluorescence detector. On using carbamate columns, the retention time was within 4 to 20 minutes. And this made it possible to separate and detect simultaneously. therefore we could analyze it exactly and efficiently and reduce time. The preparation process of MSPD method showed that the high recovery rate was more than 88.5% in most of the carbamate pesticides. Therefore we could say that it was an efficient and fast method analyzing out of lots of samples.

• Korean Journal of Veterinary Research
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• v.37 no.1
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• pp.213-220
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• 1997

A simple and rapid method known as matrix solid phase dispersion(MSPD) for simultaneous determination of 11 pesticide(2,4,5,6-tetrachlor m-xylene, ${\alpha}$-BHC, ${\gamma}$-BHC, ${\delta}$-BHC, aldrin, chlorfulazuron, heptachloroepoxide, dieldrine, endrin, endosulfan sulfate, and tetradifon) in beef fat was estabilished. Beef fat(0.5g) was fortified by adding the 11 pesticides and dibutylchlorendate as internal standard, and blended with 2g bulk $C_{18}$ in pestle and motar. Pesticides were eluted from an extraction column composed of $C_{18}$/ fat matrix blend and 2g activated Florisil by addition of 8ml acetonitrile. Then $2{\mu}l$ portion of the acetonitrile elute was directly analyzed by gaschromatography with electron capture detection. Unfortified blank control were treated similarly. Recovery rate were ranged from $83{\pm}5.4%$ to $94.2{\pm}7.6%$, intra-assay variability and inter-assay variability were ranged from 2.3% to 7.4%(n=5 for each insecticides) and from $6{\pm}1%$ to $12{\pm}3%$(n=10 for each insecticides), respectively. These results indicated that the MSPD methodology is aceptable for the extraction, determination and screening of residues 11 chroniated pesticides in beef fat.

• Korean Journal of Veterinary Research
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• v.37 no.1
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• pp.195-202
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• 1997

A method for the isolation by matrix solid phase dispersion method and liquid chromatographic determination of enrofloxacin and ciprofloxacin in pork muscle tissue is presented. Blank or enrofloxacin and ciprofloxacin spiked samples(0.5g) containing 0.05g oxalic acid were blended with $C_{18}$(octadecylsilyl derivatized silica) packing material. After homogenization, $C_{18}$/muscle tissue matrix was transferred to glass column made from 10ml glass syringe and filter paper, and compressed to 4~4.5ml volume. A column was washed with 8ml of hexane and dried under vacuum. Interfering materials were removed by ethylacetate 8ml and dried, following which enrofloxacin and ciprofloxacin were eluted with 8ml of methanal under gravity. The eluate containing enrofloxacin and ciprofloxacin wase free from interfering compound when analysed by HPLC with UV detection at 278nm. Enrofloxacin and ciprofloxacin showed linear response with UV detector at the range of $0.05{\sim}1.0{\mu}g/ml$ and eluted within 5ml elution volume of methanol from the matrix. Fortified sample containing 0.05g oxalic acid represented more good recoveries than that of control sample. Average percentages of enrofloxacin and ciprofloxacin were $93.30{\pm}4.56%$ and $91.84{\pm}4.17%$, respectively, for the concentration range(0.05, 0.1, 0.25, 0.5 and $0.75{\mu}g/g$). The interassay variability of enrofloxacin was $6.02{\pm}5.33%$ with an intra-assay variability of 4.89% and $6.75{\pm}2.68%$ with 4.54% for ciprofloxacin. Detection limit of enrofloxacin and ciprofloxacin was $0.030{\mu}g/g$ in the spiked sample.

• Analytical Science and Technology
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• v.24 no.2
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• pp.150-157
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• 2011

Aflatoxins are secondary metabolites of the molds of Aspergillus flavus and Aspergillus parasiticus. They are highly carcinogenic compounds and can affect a wide range of vegetable commodities such as cereals (especially corn), nuts, peanuts, fruits and oil seeds, in the field and during storage. In fact, oilseeds are often stored for weeks in conditions that promote the mould growth, and the possible consequent presence of aflatoxins in oilseeds can lead to their transfer in oil. In addition, aflatoxins can be found as a natural contaminant in multi-cereals and beans making baby food for infants and young-children. The objective of this study was to validate the liquid extraction method or develop an analytical method for edible oil and infant-children foods. Therefore, this study developed condition of extract for aflatoxins ($B_1$, $B_2$, $G_1$ and $G_2$) in edible oil using a high performance liquid chromatography with florescence detector (HPLC/FLD). Aflatoxins were extracted from edible oil samples by means of MSPD (Matrix solid phased dispersion), utilizing $C_{18}$ as dispersing material and purified by using immunoaffinity column. The gression line coefficients were above 0.999. The recoveries for aflatoxins ranged from 85.9 to 93.0%, and relative standard deviations were below 5.7%. The new developed method of aflatoxins effectively enhanced recoveries by using MSPD-Immunoaffinity column compared with liquid extraction. The analytical method for liquid extraction of aflatoxin was appropriate for infant-children food. Reviewing the current method, the recoveries of aflatoxins ($B_1$, $B_2$, $G_1$ and $G_2$) were 89.5~92.3%.

• Korean Journal of Veterinary Research
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• v.42 no.2
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• pp.171-181
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• 2002

Simultaneous multiresidue analysis using liquid chromatography determination for five benzimidazole anthelmintics(thiabendazole, oxibendazole, albendazole, mebendazole and fenbendazole) in bovine muscle, liver and omasum has been described. Blank or benzimidazole-fortified samples(0.5g) were blended with bulk $C_{18}$($40{\mu}m$, 18% load, endcapped, 2g). A column made from the resultant $C_{18}$/animal tissue matrix was first washed with hexane($8m{\ell}$), following which the benzimidazoles were eluted with acetonitrile($8m{\ell}$). Analytes of extracted sample were determined by liquid chromatography with UV detector at 290nm. Correlation coefficients of standard curves for individual benzimidazole isolated from fortified samples, using internal standardization, were linear($0.991{\pm}0.007$ to $0.996{\pm}0.005$) with average relative percentage recoveries from $62.1{\pm}3.8(%)$ to $92.3{\pm}7.5(%)$ for the concentration range($0.2{\sim}6.4{\mu}g/g$), respectively. Recoveries rates of TBZ, MBZ in liver, OBZ, MBZ in muscle and TBZ, MBZ in omasium from fortified benzimidazole were 92.%, 87.3%, 74.5%, 82.7%, 75.2% and 83.5% at condition II, respectively. Condition II showed higher recoveries rates than condition I. These results indicated that the matrix solid phase dispersion(MSPD) methodology is acceptable for the determination of 5 benzimidazole anthelmintics and may also suitable for other matrixes of food animal origin.

• Korean Journal of Veterinary Research
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• v.36 no.3
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• pp.541-550
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• 1996

Tetracycline antibiotics have been widely used not only therapeutics but feed additives. There are many methods for the isolation and determination of tetracycline antibiotics in animal muscle tissue. But those methods take much time and labor, so it is difficult to analyse many samples simultaneously. A rapid isolation method and liquid chromatographic determination of tetracycline antibiotics in animal muscle tissue (bovine, porcine, chicken) is presented. Blank control and tetracyclines fortified samples (0.5g) were blended with $C_{18}$ containing 0.05g each of oxalic acid and disodium ethylenediaminetetraacetate. After homogenize, homogenate was transferred to glass column made from 10ml glass syringe and compressed to 4~4.5ml volume. A column made from the $C_{18}$/meat matrix was washed with hexane (8ml) and dichloromethane (8ml, if needed), following which the tetracyclines were eluted,vith methanol or 0.01M methanolic oxalic acid (8ml). The eluates containing tetracyclines analytes were free from interfering compounds when analysed by HPLC with UV detection (photodiode array at 360nm). Standard curve for each tetracycline showed a linear response at the range of $0.05{\sim}1.0{\mu}g/ml$ and tetracycline antibiotics were eluted within 4ml of eluted volume. All tetracycline antibiotics except tetracycline were stable during the concentration process at $40^{\circ}C$ and time required for concentration was 3~4 hours. Fortified samples containing oxalic aicd and EDTA represented more good recoveries than those of not-contained sample. Recoveries were 91.8~110.1% (oxytetracycline; OTC), 57.7~79.5% (tetracycline; TC), 78.1~88.6% (chlortetracyclines; CTC) and 88.4~100.6% (doxycycline; DC) in pork tissue, 101.1~126.8% (OTC), 66.4~75.4% (TC), 79.2~88.1% (CTC) and 69.3~86.7% (DC) in beef tissue, and 90.8~95.6% (OTC), 66.2~84.4% (TC), 75.7~77.2% (CTC) and 55.6~80.7% (DC) in chicken muscle tissue. The detection limits validated in muscle tissue by this method were $0.05{\mu}g/g$ for OTC and TC, and $0.1{\mu}g/g$ for CTC and DC.