• Title/Summary/Keyword: sulfonamides

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Simultaneous analysis of sulfonamides in beef and pork by high performance liquid chromatography and electrospray ionization mass spectrometry (HPLC와 LC/MS에 의한 식육내 잔류 설파제의 동시 분석법)

  • 정봉수;박준조;금모래;김인경;박병옥;한정희
    • 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.

A Study on Detection Method of Sulfonamides Residues in Raw Milk by HPLC (HPLC를 이용한 원유중 잔류 Sulfonamides 분석법 연구)

  • 정동수;윤교복;김종술;신명균;김교승
    • Korean Journal of Veterinary Service
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    • v.16 no.1
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    • pp.11-19
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    • 1993
  • This experiment was carried out to detect the residues of sulfonamides in raw milk. Raw milks which does not contain sulfonamides was collected from one of the farm and fortified with 5 sulfonamides (sulfamerazine, sulfamethazine, sulfamonomethoxine, sulfadimethoxine, sulfaqinoxaline). The sulfonamides in the fortified sample were extracted and detected by High Performance Liquid Chromatography. UV /vis detector was used in this experiment. The results obtained were summarized as follows : 1. Chloroform was good as a extracting solution. 2. 15.5% methanol in PDP as a mobile phase solution was best detective condition for SMR, SMT, SMM. But for SDM and SQN the best condition was 23% methanol. 3. The detectable limits of SMR, SMT, SMM were 2ppb. but SDM and SQN were 20ppb because of delayed retention time and relatively low recovery rate. 4. The peaks of SMR, SMT, SMM and SDM were erected at baseline and the apexes were sharp but SQN was round shape.

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Determination of Sulfonamides in Meat by Liquid Chromatography Coupled with Atmospheric Pressure Chemical Ionization Mass Spectrometry

  • Kim, Dal-Ho;Choi, Jong-Oh;Kim, Jin-Seog;Lee, Dae-Woon
    • Bulletin of the Korean Chemical Society
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    • v.23 no.11
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    • pp.1590-1594
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    • 2002
  • Liquid chromatography/atmospheric pressure chemical ionization-mass spectrometry (LC-APCI-MS) has been used for the determination of sulfonamides in meat. Five typical sulfonamides were selected as target compounds, and beef meat was selected as a matrix sample. As internal standards, sulfapyridine and isotope labeled sulfamethazine (${13}^C_6$-SMZ) were used. Compared to the results of recent reports, our result have shown improved precision to a RSD of 1.8% for the determination of sulfamethazine spiked with 75 ng/g level in meat.

Survey on the residual drugs (tetracyclines, ${\beta}$-lactams, chloramphenicol, sulfonamides) on beef and pork carcass at abattoir in Seoul (서울 시내 도축장의 소${\cdot}$돼지 지육에 대한 잔류물질 (tetracyclines, ${\beta}$-lactams, chloramphenicol, sulfonamides) 함량 조사)

  • Kim Doo-Hwan;Lee Jae-Shin;Ham Hee-Jin;Ki No-Joon;Lee Jung-Hark
    • Korean Journal of Veterinary Service
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    • v.27 no.3
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    • pp.265-272
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    • 2004
  • It was carried out to compare the residual materials by EEC 4-plate, Charm II and HPLC method in the muscles of cattle and pigs from slaughter-houses in Seoul from 2000 to 2003. Residual materials were detected from $1.10\%$(73/6,623) samples by EEC 4-plate method, and $10.93\%$(55/503) samples by Charm II method. The highest residual concentration(ppm) of oxytetracycline, tetracycline, chloramphenicol, chlortetracycline, sulfamethazine, sulfamerazine, sulfadimethoxine, penicillin and sulfamonomethoxine were 25.5, 3.46, 3.26, 1.5, 0.3, 0.2, 0.2, 0.14, and 0.07, respectively. Eighty nine samples were classified as 58($65.17\%$) only tetracyclines, 20($22.47\%$) only sulfonamides, 3($3.37\%$) only ${\beta}$-lactams, 2($2.25\%$) only chloramphenicol, 4($4.49\%$) tetracyclines and sulfonamides simultaneously, 1($1.12\%$) chloramphenicol and sulfonamides simultaneously, and 1($1.12\%$) chloramphenicol, sulfonamides and tetracyclines simultaneously.

Investigation of residual levels and pertaining detection wavelength of 5 sulfonamides in the mouse muscle (마우스 근육내 설파제 잔류량조사 및 동시분석파장 연구)

  • Chung, Kyung-Tae;Cho, Hyun-Ho;Lee, Gang-Rog;Lee, Woo-Won;Yang, Ju;Kim, Geun-Kyu
    • Korean Journal of Veterinary Service
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    • v.21 no.4
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    • pp.379-383
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    • 1998
  • This survey was carried out to determine 5 residual sulfonamides(sulfamerazine : SMR, sulfamethazine : SMT, sulfamonomethoxine : SMM:, sulfadimethoxine : SDM, sulfaquinoxaline : SQX) in muscle of mouse. For this investigation, pertaining detection wavelength, residual levels and residual times in muscle of mouse were summarized as follows ; 1. Pertaining detection wavelength of 5 residual sulfonamides(SMR, SMT, SMM, SDM, SQX) was 270nm by HPLC/UV detection. 2. After 1 day put a stop to sulfonamides administration, residual levels was 1∼l.5ppm, but were not detected at day 7 3. Withdrawal time of 5 sulfonamides were about 7 days suspectly.

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An experimental study on the comparison of trace amount of sulfonamides detection method in raw milk. (원유중 미량 설파제 검출방법 비교에 대한 실험적 연구)

  • 황원무;이성모;손봉환;이원창
    • Korean Journal of Veterinary Service
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    • v.20 no.1
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    • pp.79-93
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    • 1997
  • The sulfonamide is one of potentiative antimicrobial agents which is being used widely in veterinary medicine for control of several animal diseases such as mastitis as well as for promotion of growth. However, the misusages of sulfonamides in food producing animals, especially cattle produce several considerable problems in human health caused from residues of this antibiotic in milk product. To determine the most effective analytical methods for residual sulfonamides in raw milk, this study was performed comparatively using by some applicable screening detecting method such as TTC, Charm II test (sulfonamides), and Lactek tests (sulfamethazine kit). The positive result from screening tests was confirmed by HPLC method. Milk samples (540 raw milks) were collected from dairy farms. Results of this study are summariezed as follorrs ; 1. All samples (540 raw milks) showed negative response from TTC test, however, 18 raw milks of those samples responded positively to Charm II test. 2. By Lactek test, residual sulfamethazine was detected from 4 raw milks. Fifteen raw milks of 18 samples which were classified as positive one by Charm II test, showed positive response 3. Retention time of sulfonamides added at the level of 100ppb into sklm milk was ranged from 1.55 minute to 23.3 minute. Recovery rates of sulfonamides were variable from 6.7% upto 94.2% depended on the types of sulfonamlde. 4. Single type of sulfonamides was detected from 10 raw milk samples, 2 types of sulfonamides from 3 samples and 3 types from 2 raw milks by HPLC. 5. Sulfonamides was detected in this study were 5 types : 11 samples for sulfisomidine, 5 samples for sulfamethazine, 3 samples for sulfadlmethoxine, 2 samples for sulfathiazole and 1 sample for sulfadiazine. 6. The highest levels of residual sulfonamides was 210.3 ppb of sulfamethazine but the lowest concentration of residue was 2.2 ppb of sulfamethazine and sulfisomidine, respectively. Number of samples detected positively in this experiment were belows : above 100 ppb for 1 sample (4.5%) (sulfamethazine), 50~100 ppb for 4 samples (18.1%) (each 2 samples for sulfamethazine and sulfisomidine, respectively), 25~50 ppb for 6 samples (27.1%) (2 sulfisomidine, each 1 sample for sulfadiazine, sulfadimethoxine, sulfamethazine and sulfathiazole, respectively), 10~25ppb for 3 samples (13.7%) (3 sulfisomidine), and below 10ppb for 8 samples (36.4%) (4 sulfisomidine, 2 sulfadimethoxine and each 1 for sulfamethazine and sulfathiazole).

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Spectrofluometry of sulfonamides using fluorescamine (Fluorescamine을 이용한 sulfonamide의 형광 분석법)

  • Lim, Jae-young;Han, Su-nam;Lee, Mun-han;Park, Jong-myung
    • Korean Journal of Veterinary Research
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    • v.30 no.1
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    • pp.41-49
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    • 1990
  • These experiments were carried out to develop a novel, simple, and rapid method to determine urinary sulfonamides using fluorescamine by spectrofluorometry. To get optimal conditions for the sulfonamide-fluorescamine reaction, sulfonamides such as sulfamethazine, sulfamerazine, sulfadimethoxine and sulfamonomethoxine, dissolved in buffers with various pH ranges were reacted with various concentrations of fluorescamine. and then, the fluorescence intensity and stability of the fluorophore were measured. To eliminate the interfering substances in urine, the fluorophore in buffers and urine with a definite pH range was extracted with some organic solvents. After then the fluorescence intensity was measured in organic and aquous phases. The results obtained were summarized as follows: 1. The maximal fluorescence of sulfonamides was presented in acidic state, pH 4.5~5.0, at 30 minutes after reaction. 2. The optimal concentration ratio of sulfamethazine and ffuorescamine was more than 1 : 40 in mole. 3. In pH 4.0, the intensity was maximal but was time-dependent, whereas in pH 8.0, the intensity was time-independent. 4. Sulfamethazine-fluorescamine conjugate could be dissolved in some of organic solvents in acidic state such as chloroform, n-butanol, and ethylacetate. 5. Sulfamethazine-flnorescamine conjugate in swine urine coule be extracted with ethylacetate in acidic state, pH 4.0~5.0.

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Cytotoxicities and Quantitative Structure Activity Relationships of B13 Sulfonamides in HT-29 and A549 Cells

  • Lee, Seul Ki-Chan;Park, Sang-Min;Im, Chae-Uk
    • The Korean Journal of Physiology and Pharmacology
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    • v.15 no.6
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    • pp.423-429
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    • 2011
  • B13 analogues are being considered as therapeutic agents for cancer cells, since B13 is a ceramide analogue and inhibits ceramidase to promote apoptosis in cancer cells. B13 sulfonamides are assumed to have biological activity similar to B13, since they are made by bioisosterically substituting the carboxyl moiety of B13 with sulfone group. Twenty B13 sulfonamides were evaluated for their in vitro cytotoxicities against human colon cancer HT-29 and lung cancer A549 cell lines using MTT assays. Replacement of the amide group with a sulfonamide group increased cytotoxicity in both cancer cell lines. The sulfonamides with long alkyl chains exhibited activities two to three times more potent than that of B13 and compound (15) had the most potent activity with $IC_{50}$ values of 27 and $28.7{\mu}M$ for HT-29 and A549, respectively. The comparative molecular field analysis (CoMFA) and comparative molecular similarity indices analysis (CoMSIA) were used to carry out QSAR molecular modeling of these compounds. The predictive CoMSIA models for HT-29 and A549 gave cross-validated q2 values of 0.703 and 0.830, respectively. From graphical analysis of these models, we suppose that the stereochemistry of 1,3-propandiol is not important for activity and that introduction of a sulfonamide group and long alkyl chains into B13 can increase cytotoxicity.

Convenient One-Pot Synthesis of Sulfonamides from Thiols and Disulfides Using 1,3-Dichloro-5,5-dimethylhydantoin (DCH)

  • Veisi, Hojat
    • Bulletin of the Korean Chemical Society
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    • v.33 no.2
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    • pp.383-386
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    • 2012
  • A convenient synthesis of sulfonamides from thiols and disulfides is described. In situ preparation of sulfonyl chlorides from thiols is accomplished by oxidation with 1,3-dichloro-5,5-dimethylhydantoin (DCH) under Nbenzyl-trimethylammonium chloride and water. The sulfonyl chlorides are then further allowed to react with excess amine in the same reaction vessel.

Studies on the effect of various para-sympatholytic agents to the absorption of some sulfanamides (부교감신경차단성약물이 sulfa제의 흡수에 미치는 영향에 관한 연구)

  • 김재완
    • YAKHAK HOEJI
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    • v.12 no.1_2
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    • pp.16-31
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    • 1968
  • Comparative studies were made on some sulfonamides, used individually and combined with parasympatholytic agents as regards (1) the absorption rate through isolated rat small intestine (in vitro), (2) the absorption rate through rat small intestine (in vivo), and (3) the blood concentration of sulfonamides were examined by its oral administration with each combined drug to rabbits, and the following effects were found, parasympatholytic agents inhibit the absorption of sulfonamides from the small intestinal tract. Comparison of the inhibitic efficiency of parasympatholytic agents is as follows: oxazepam, oxyphencyclimine hydrochloride, probantheline bromide, atropine sulfate (The examples are from the weakest to the strongest). Decrement of the absorption rate of sulfonamides is as follows: sulfadiazine, sulfathiazole, sulfamethoxypyridazine, sulfadimethoxine, sulfamerazine, sulfamethazine (The example are from the strongest to the weakest). Additionally, it is assumed that if the combined drugs were absorbed from the small intestine in the original form, those inhibitic effects should be best regarding to their sulfonamide per parasympatholytic agent combined rate "25:1" than to their any other rates.her rates.

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