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PubMed2005

Evaluating the biodegradability of sulfamethazine, sulfamethoxazole, sulfathiazole, and trimethoprim at different stages of sewage treatment.

The aerobic biodegradability of four antimicrobials (sulfamethazine, sulfamethoxazole, sulfathiazole, and trimethoprim) was investigated in sewage collected at four treatment stages (primary treatment, activated sludge treatment, aerobic nitrification process, and after disinfection of treated sewage) of a municipal sewage treatment plant. The biodegradability tests were conducted in aerated batch reactors by spiking the sewage with 20 microg/L of each of the test substance. Concentration profiles of the assayed compounds were monitored during a 54-d period using liquid chromatography/electrospray ionization/mass spectrometry. Substantial differences in the degradation curves were observed between trimethoprim and the three sulfonamides. The behavior of the latter was characterized by a general biodegradability in the primary and secondary treatment. The highest degradation rates were obtained in the sewage from the activated sludge treatment, where no adaptation phase was observed. On the other hand, the onset of biodegradation in the sewage from the primary treatment was preceded by a lag phase ranging from 10 to 15 d. In contrast, trimethoprim displayed high resistance to microbial degradation in the sewage from the primary treatment and the activated sludge treatment. However, primary degradation of this compound was completed within only 3 d in the sewage from the nitrification process.

Biodegradation, Environmental↗
PubMedDate not supplied

Determination of sulfathiazole in type C medicated swine feed by reversed-phase liquid chromatography with post-column derivatization.

A convenient method was developed for determination of sulfathiazole (STZ) in Type C medicated swine feed by reversed-phase liquid chromatography (LC) with post-column derivatization. Addition of extractant solution (0.2N HCl and 1.5% diethylamine in 25% methanol) and an internal standard (IS), sulfamethylthiazole (SMZ), to 5 g sample was followed by mechanical shaking for 1 h. The extract was clarified by chilling, centrifugation, and filtering before injection onto a C18 reversed-phase column. The mobile phase components were 2% acetic acid and 1:1 acetonitrile-methanol (83 + 17%, v/v). Run time was about 20 min. Determination and, largely, the method's selectivity were based on detection at 450 nm of the derivative formed by the post-column reaction of dimethylaminobenzaldehyde with the primary amine of the analyte and IS. The IS, SMZ, differs from STZ by a single substituent methyl group, is stable, and is readily resolved from STZ. Although SMZ is not commercially available, it can be synthesized with relative ease from purchased reagents and will be supplied by the authors to interested laboratories. In single-laboratory validation, linearity was demonstrated over the range of 0.055-550 microg/mL, well beyond the target concentration of 5.5 microg/mL. The estimated limit of detection was 0.04 microg/mL; the calculated limit of quantitation was 0.13 microg/mL (feed concentration of 2.4 g/T or 2.7 mg/kg). Wet-spiking trials with a variety of swine feed matrixes showed recovery to be 100-102% for the intended concentration range, 50-200 g/T, with coefficient of variation (CV) < 2%. The method ruggedness was verified with an overall CV of 2.9%.

Animal Feed↗
PubMedDate not supplied

Confirmation of sulfamethazine, sulfathiazole, and sulfadimethoxine residues in condensed milk and soft-cheese products by liquid chromatography/tandem mass spectrometry.

A liquid chromatography/tandem mass spectrometry method (LC/MS/MS) is described for the simultaneous detection of 3 sulfonamide drug residues at 1.25 ppb in condensed milk and soft-cheese products. The 3 sulfonamide drugs of interest are sulfathiazole (STZ), sulfamethazine (SMZ), and sulfadimethoxine (SDM). The method includes extraction of the product with phosphate buffer, centrifugation of the diluted product, and application of a portion of the extract onto a polymeric solid-phase extraction cartridge. The cartridge is washed with water, and the sulfonamides are eluted with methanol. After evaporation, the residue is dissolved in 0.1% formic acid solution, and the solution is filtered before analysis by LC/MS/MS. The LC/MS/MS program involved a series of time-scheduled selected-reaction monitoring transitions. The transitions of MH+ to the common product ions at m/z 156, 108, and 92 were monitored for each residue. In addition, SMZ and SDM had a fourth significant and unique product ion transition that could be measured. Validation was performed with control and fortified-control condensed bovine milk with 2.5, 5, and 10 ppb sulfonamides. This method was applied to imported flavored and unflavored condensed milk and cream cheese bars. The presence of STZ and SMZ residues was confirmed in 3 out of 6 products.

Animals↗
PubMed1990

Effect of Haemonchus contortus infection on the clearance of antipyrine, sulfobromophthalein, chloramphenicol, and sulfathiazole in lambs.

A study was made to determine the effect of Haemonchus contortus parasitic infection in lambs on the clearance of several IV administered drugs. Clearance of sulfobromophthalein or sulfathiazole from the plasma of lambs was unaffected by infection with H contortus. Clearance of antipyrine was enhanced by the infection, and thiabendazole treatment did not alter this effect. Clearance of chloramphenicol (CAP), administered as the succinate ester (CAPS), was not changed by the infection, but it was increased after treatment with thiabendazole. Changes in the mean body residence time and initial plasma concentration of CAPS and CAP after treatment with thiabendazole indicate that hydrolysis of CAPS to CAP was reduced. High concentrations of CAPS apparently enhanced its own elimination directly rather than via the expected sequence involving hydrolysis, glucuronidation, and excretion of CAP-glucuronide. Enhanced clearance of antipyrine following infection of lambs with H contortus can be explained in at least 2 ways. First, it is possible that the lambs did not have mature amounts of hepatic drug metabolizing enzyme activity as reported by other investigators, which may be explained by breed differences or animal husbandry practices. Second, infection of lambs by H contortus may have triggered an inductive response in hepatic cytochrome P-450-mediated activities, which might result via a generalized enhancement in hepatic protein synthesis associated with the physiologic response to replace plasma proteins and other blood components lost through gastrointestinal hemorrhage caused by the active feeding of adult worms. Other phase-II reactions such as acetylation, glucuronidation, and glutathione-S-transferase apparently were not affected.

Animals↗
PubMedDate not supplied

Enzyme immunoassay for screening of sulfathiazole in honey.

A simple enzyme immunoassay (EIA) was developed to screen honey samples for sulfathiazole (ST) adulteration. Honey samples required only a 30-fold dilution before use in the procedure. Because 96 well microtiter plates were used and only 100 microL of diluted honey sample was required per well, numerous replicates or samples could be tested simultaneously. The EIA was able to detect at least 0.3 ppm levels of ST in honey and also provide a rough quantitation of ST amounts.

Drug Residues↗
PubMedDate not supplied

Sulfamethazine and sulfathiazole determination at residue levels in swine feeds by reverse-phase liquid chromatography with post-column derivatization.

Twenty g sample, to which sulfamerazine has been added as internal standard, is extracted with 0.3N HCl + 1.5% diethylamine in 25% methanol. The sample extract is chilled (to aid clarification), centrifuged, and filtered. The sulfonamides are separated from each other and from co-extracted materials on a C-18 reverse-phase column and detected at 450 nm following post-column derivatization with dimethylaminobenzaldehyde. Two isocratic mobile phases have been tested: (1) acetonitrile-2% acetic acid (17 + 83), with an analysis time of 13 min; and (2) acetonitrile-methanol-2% acetic acid (4 + 16 + 80), with an analysis time of 20 min but an improved analysis for some samples. As many as 40 samples have been analyzed at one time unattended with the aid of an autosampler. A total of about 1500 field samples have been assayed using the method. Method sensitivity is 0.1 ppm for either analyte in a hog finishing fed. Linearity for each of the analytes is satisfactory over a range of 0.4-25 ppm in spiked feeds. Coefficients of variation range from 13% at 0.5 ppm to 2% at 13 ppm as tested over a period of time in naturally contaminated samples. The absolute recovery of sulfamerazine varies with sample matrix, but, in the presence of sulfamerazine as internal standard, recovery has been 96.7-99.7% over the range of 0.1-10 ppm. Sulfamerazine and sulfamoxole were tested for their suitability as internal standards. Sulfamerazine is a good internal standard for sulfamethazine; neither is ideal for sulfathiazole.(ABSTRACT TRUNCATED AT 250 WORDS)

Animal Feed↗
PubMedDate not supplied

Practical screening procedure for sulfathiazole in honey.

A simple, inexpensive procedure is described for rapidly screening small samples of honey for sulfathiazole (ST), a drug formerly used but not approved in the United States for the prophylactic treatment of American foulbrood disease of bees. The method uses 2 plastic tubes arranged in tandem. The upper tube contains a bed of alumina, which removes some interfering pigments. The lower tube contains a very small bed of anion exchange resin in the HSO4- form, which traps the ST. The drug is eventually eluted and detected using the Bratton-Marshall diazotization-coupling reagents. Honey containing 0.1 ppm ST can be readily detected. An optional dye concentration step permits the detection of as little as 25 ppb ST.

Chromatography, Ion Exchange↗
PubMedDate not supplied

Bioavailability of sulfathiazole from flocculated and deflocculated suspensions and its implications.

Flocculation is commonly used to stabilize pharmaceutical suspensions. Flocculated and deflocculated suspensions of sulfathiazole were administered to healthy human volunteers. Bioavailability from these two types of suspensions was studied from urinary free drug excretion. Bioavailability was significantly lower from flocculated suspensions. The study indicates the necessity of studying all flocculated drug suspensions for bioavailability data.

Biological Availability↗
PubMed1983

Rapid gas-liquid chromatographic method for determination of sulfathiazole in swine feed.

A gas-liquid chromatographic (GLC) method for determining residues of sulfathiazole (STZ) in swine feed has been developed. Feed is extracted first with acetone and then with ammonia-acetone. STZ is isolated from other feed extractives on a Sephadex LH-20 column with methanol-toluene. The sulfa residues are methylated with diazomethane, and the eluate is evaporated to dryness. A solution containing an internal standard of methyl sulfasymazine is used to dilute the sample before injection onto an OV-25 GLC column. The precision of the method was determined by assaying 10 sets of feed spiked at 0.5, 1, 2, and 5 ppm STZ. The mean recoveries and coefficients of variation were 90.2 (5.90), 89.5 (4.67), 87.4 (5.62), and 87.7% (4.29), respectively. The critical steps of the method, including the stability of STZ, were also determined.

Animal Feed↗
PubMed1982

Use of post-column derivatization in liquid chromatographic determination of sulfamethazine and sulfathiazole in feeds and feed premixes.

Sulfonamide drugs are extracted from feed and feed premixes by shaking with 0.15N HCl in 25% methanol. The extract is diluted, clarified, and chromatographed on a reverse phase C18 column. Mobile phases used are methanol-2% acetic acid (35 + 65) and acetonitrile-2% acetic acid (18 + 82) for sulfamethazine (SMT) and sulfathiazole (STZ), respectively. A solution of dimethylaminobenzaldehyde (DMAB) is added to the column eluate and the resulting sulfonamide-DMAB complex is detected at 450 nm. The method was tested for linearity, recovery, and precision across a broad sample range. Recovery was 100.6 +/- 2.3% and 96.3 +/- 1.6% for STZ and SMT, respectively. Linearity was excellent (r2 = 0.9985 for STZ and r2 = 0.9996 for SMT) as was within-day precision (RSD = 2.00% for STZ and 1.52% for SMT). The method was compared with the Bratton-Marshall colorimetric method. Analysis of 14 STZ and 15 SMT samples failed to detect any bias between the 2 methods. Some practical aspects of the use of this technique are discussed.

Animal Feed↗
PubMed1976

Effect of polyethylene glycol 4000 on dissolution properties of sulfathiazole polymorphs.

The dissolution rates of the two polymorphic forms of sulfathiazole containing polyethylene glycol 4000 were significantly different in water. The effect of agitation on the dissolution rates also was studied. At higher stirring speeds, the dissolution rates of the stable form were affected more than the metastable form. A high concentration of polyethylene glycol 4000 seemed to affect the dissolution properties of the metastable polymorph more than the stable polymorph.

Isomerism↗
PubMed1976

Enhancement of dissolution rates of poorly water-soluble drugs by crystallization in aqueous surfactant solutions I: Sulfathiazole, prednisone, and chloramphenicol.

Effects of crystallization of poorly water-soluble drugs in aqueous surfactant solution on in vitro dissolution rates were investigated. Marked enhancement was observed for chloramphenicol, sulfathiazole, and prednisone. Differential thermal analysis studies indicated the presence of small amounts of surfactant in surfactant-treated crystals. Possible mechanisms of dissolution enhancement are discussed.

Chemistry, Pharmaceutical↗
PubMed1977

Direct spectrophotometric determination of sulfathiazole in presence of sulfadiazine and sulfamerazine.

A direct spectrophotometric method for the quantitative determination of sulfathiazole and the total pyrimidyl sulfonamide content in a mixture containing sulfadiazine and sulfamerazine is reported. This three-component system was readily reduced to the problem of a simple two-component system analysis. Based on dual isoabsorptive wavelength spectroscopy, simultaneous equations were developed that required absorbance measurements at only two selected wavelengths both isoabsorptive. The location of the isoabsorptive wavelengths was dependent on the pH of the solvent medium, and 0.1 M HCl gave the best results. The validity of the derived equations was demonstrated in a recovery study involving synthetic mixtures containing varying quantities of the three sulfonamides. The recovery was linear over a wide concentration range, and the precision of the method was about 1%.

Methods↗
PubMed1976

Histological studies of the effects of subperiosteally implanted sulfathiazole.

The use of implanted sulfathiazole to obliterate undercut alveolar ridges has given good results. The mechanism whereby this drug effects this change has been investigated with dogs as experimental models. It was found that a fibroplastic proliferation occurred that was possibly due to an irritative stimulus on the periosteum.

Alveolar Process↗
PubMedDate not supplied

Confirmation of identity by gas chromatography/tandem mass spectrometry of sulfathiazole, sulfamethazine, sulfachloropyridazine, and sulfadimethoxine from bovine or swine liver extracts after quantitation by gas chromatography/electron-capture detection.

Four sulfonamide veterinary drug residues were quantitated by electron-capture detection (ECD) after separation by gas chromatography (GC). The identities of sulfathiazole (ST), sulfamethazine (SM), sulfachloropyridazine (SCP), and sulfadimethoxine (SDM) were confirmed in bovine or swine liver residues by tandem mass spectrometry (MS/MS). Bovine or swine liver tissues were extracted by using either the Tishler or the Manuel-Steller cleanup. The methylated residues containing ST, SM, SCP, and SDM were separated by GC prior to MS/MS daughter ion analysis. Control tissue, control tissue fortified at 0.1 ppm, and incurred tissue residues at approximately 0.1 ppm were analyzed for these 4 sulfonamides. A Finnigan Model TSQ-46 operating in the chemical ionization mode was used to perform the MS/MS daughter ion experiments. The identities of all 4 sulfonamides were confirmed in a single GC/MS/MS analysis.

Animals↗
PubMed1983

[Influence of the pressing force on the physical features of sulfathiazole tablets and the dissolution rate of the active ingredient].

When the pressing force increased in the examined system, so did the mechanical firmness of the tablets. A logarithmic connection exists between the pressing force and the compression strength and between the pressing force and the porosity, while the connection between the pressing force and the abrasion loss was a connection of power-function. The changing of the pressing force don't alter significantly the disintegration time of the tablets and the dissolution rate of the drug. However there is a considerable difference between the dissolution rate of the sulfathiazolee-powder and that of the tablets. The binders used in the pressing process were surface-active, therefore they accelerated the dissolution by moistening the surface of the sulfathiazol crystals.

Drug Compounding↗
PubMed1983

Reverse phase liquid chromatographic determination of sulfathiazole residues in honey.

Sulfathiazole residues were extracted from honey by homogenizing samples in acetone, filtering, and then evaporating the acetone under nitrogen at 40 degrees C. The remaining extract was transferred to a separatory funnel with 1N HCl and ethyl ether. An aliquot of the retained acid layer was screened by using the Bratton-Marshall reaction. If the test was positive, the remaining portion was analyzed directly through a mu Bondapak phenyl column monitored by a UV detector at 254 nm. The mobile phase was potassium phosphate monobasic in 10% acetonitrile adjusted to pH 3.0. Time for elution was 13 min. Average recoveries were 78% at the 0.1 ppm spiking level and 68% at the 1.0 ppm level. The minimum detectable amount was 0.06 ppm based on a spiked sample extract.

Chromatography, High Pressure Liquid↗