Tissue distribution, metabolism, and residue depletion study in Atlantic salmon following oral administration of [3H]emamectin benzoate

Atlantic salmon (approximately 1.3 kg) maintained in tanks of seawater at 5 +/- 1 degrees C were dosed with [3H]emamectin B1 benzoate in feed at a nominal rate of 50 microg of emamectin benzoate/kg/day for 7 consecutive days. Tissues, blood, and bile were collected from 10 fish each at 3 and 12 h and at 1, 3, 7, 15, 30, 45, 60, and 90 days post final dose. Feces were collected daily from the tanks beginning just prior to dosing to 90 days post final dose. The total radioactive residues (TRR) of the daily feces samples during dosing were 0.25 ppm maximal, and >97% of the TRR in pooled feces covering the dosing period was emamectin B1a. Feces TRR then rapidly declined to approximately 0.05 ppm by 1 day post final dose. The ranges of mean TRR for tissues over the 90 days post dose period were as follows: kidney, 1.4-3 ppm; liver, 1.0-2.3 ppm; skin, 0.04-0.09 ppm; muscle, 0.02-0.06 ppm; and bone, <0.01 ppm. The residue components of liver, kidney, muscle, and skin samples pooled by post dose interval were emamectin B1a (81-100% TRR) and desmethylemamectin B1a (0-17% TRR) with N-formylemamectin B1a seen in trace amounts (<2%) in some muscle samples. The marker residue selected for regulatory surveillance of emamectin residues was emamectin B1a. The emamectin B1a level was quantified in individual samples of skin and muscle using HPLC-fluorometry and was below 85 ppb in all samples analyzed (3 h to 30 days post dose).     

Residue depletion of tilmicosin in cattle after subcutaneous administration

A study of tissue residue depletion of tilmicosin in cattle was conducted after a single subcutaneous injection at the therapeutic level of 10 mg per kg body weight. Eighteen cross cattle were treated with the tilmicosin oil formulation (30%). Three treated animals (two males and one female) were selected randomly to be scarified at 1, 7, 14, 28, and 35 days withdrawal after injection. Samples of the injection site and of muscle, liver, kidney, and fat were collected. Tilmicosin residue concentrations were determined using a high-performance liquid chromatography (HPLC) method with a UV detector at 290 nm. Using a statistical method recommended by the Committee for Veterinary Medical Products of European Medical Evaluation Agency, the withdrawal time of 34 days was established when all tissue residues except samples in the injection site were below the accepted maximum residue limits.     

Residue depletion of nitrovin in chicken after oral administration

In this study, the residue depletion of nitrovin in chicken was studied after feeding the birds with dietary feeds containing 10 mg/kg of nitrovin for 7 consecutive days. Tissues (muscle, fat, kidney, and liver) and plasma were collected at different withdrawal periods and determined by a high-performance liquid chromatography-ultraviolet (HPLC-UV) method. The limit of detection for nitrovin in tissue and plasma samples was 0.1 ng/(g or mL), and the inter- and intrarecoveries from the blank fortified samples were in the range of 71.1-85.7%. At the withdrawal period of 0 days, the residue concentration of nitrovin in plasma was the highest (average of 84.98 ng/mL) compared to those in muscle, fat, liver, and kidney (average of 21.04, 61.18, 24.04, and 68.28 ng/g, respectively). At the withdrawal period of 28 days, the residue levels of nitrovin in muscle, fat, liver, and plasma were all higher than 1.0 ng/(g or mL) and the highest concentration was in liver (average of 5.8 ng/g). These data are in support of the ban of nitrovin as a feed additive in food-producing animals.     

Residue depletion of cefquinome in swine tissues after intramuscular administration

A high-performance liquid chromatography (HPLC) method with ultraviolet (UV) detection was developed for the detection of cefquinome (CEQ) residues in swine tissues. The limit of detection (LOD) of the method was 5 ng g(-1) for muscle and 10 ng g(-1) for fat, liver, and kidney. Mean recoveries of CEQ in all fortified samples at a concentration range of 20-500 ng g(-1) were 80.5-86.0% with coefficient of variation (CV) below 10.3%. Residue depletion study of CEQ in swine was conducted after five intramuscular injections at a dose of 2 mg kg(-1) of body weight with 24 h intervals. CEQ residue concentrations were detected in muscle, fat, liver, and kidney using the HPLC-UV method at 265 nm. The highest CEQ concentration was measured in kidney tissue during the study period, indicating that kidney was the target tissue for CEQ. CEQ concentrations in all examined tissues were below the accepted maximum residue limit (MRL) recommended by the Committee for Veterinary Medical Products of European Medical Evaluation Agency (EMEA) at 3 days post-treatment.     

Residue depletion of eprinomectin in bovine tissues after subcutaneous administration

A study of the tissue depletion of eprinomectin (EPR) subcutaneously administered to cattle at a dose of 500 mg per kg of body weight was carried out. EPR concentrations were determined in muscle, liver, kidney, and fat. Twenty-four parasite-free cross cattle were treated with the EPR injectable oil formulation. Three treated animals (two males and one female) were selected randomly to be sacrificed at 1, 3, 7, 14, 21, 28, 42, and 56 days withdrawal after injection. EPR residue concentrations were determined using HPLC with fluorescence detection. Muscle samples showed the lowest EPR concentrations throughout the study period. The highest EPR concentrations at all sampling times were measured in liver tissue, indicating that liver is a target tissue for EPR. EPR concentrations in all of the tissues analyzed were below the accepted maximum residue limits recommended by the European Union at 8 days posttreatment.     

Quantitative analysis of tylosin in eggs by high performance liquid chromatography with electrospray ionization tandem mass spectrometry: residue depletion kinetics after administration via feed and drinking water in laying hens

Maximum residue limits (MRLs) have been established by the European Union when tylosin is used therapeutically. They are fixed at 200 microg/kg for eggs. A highly sensitive and selective quantitative liquid chromatography electrospray ionization tandem mass spectrometry (LC/ESI/MS/MS) method suitable for monitoring tylosin residues in eggs to determine its depletion kinetics was developed and validated. For sample pretreatment all samples were liquid-liquid extracted with citrate buffer (pH 5.0) and acetonitrile. Liquid chromatographic separation was carried out on a reversed phase C18 column employing a 0.5% formic acid/acetonitrile gradient system. The tylosin recovery in eggs at a concentration range from 1.0-400 microg/kg was >82% with relative standard deviations between 1.5 and 11.0%. In two experimental studies administrating tylosin via feed (final dosage: 1.5 g/kg) or drinking water (final dosage: 0.5 g/L), no residues above the MRL were found during and after treatment. Moreover, all samples were well below the actual MRL of 200 microg/kg. Therefore, our residue data suggest that a withholding period for eggs is not required when laying hens are treated with tylosin in recommended dosages via feed or drinking water. Keywords: Tylosin; residue; depletion; laying hen; withholding period; mass spectrometry.     

Residue depletion of florfenicol and its metabolite florfenicol amine in Swine tissues after intramuscular administration

A study of the tissue depletion of florfenicol (FF) administered intramuscularly twice to swine at a dose rate of 20 mg per kg of body weight at 24 h intervals was carried out. Forty healthy cross swine were treated with the FF injection formulation. Five treated animals were selected randomly to be sacrificed at 1, 3, 6, 9, 12, 14, 17, and 21 days withdrawal. FF and florfenicol amine (FFa) residue concentrations in muscle, liver, and kidney were determined using high-performance liquid chromatography (HPLC) with photodiode array (PDA) detection at 225 nm. Liver samples showed the lowest FF and the highest FFa concentrations throughout the experiment period. However, the highest total concentrations of FF and FFa during the study were found in kidney, which indicated that kidney is the target tissue for FF. The sum of FF and FFa concentrations in all tissues analyzed was below the accepted maximum residue limits recommended by the Agriculture Ministry of People's Republic of China and the European Union at 8 days posttreatment.     

挤压豆渣中可溶性膳食纤维制备工艺的优化

为了获得碱法制备挤压豆渣中可溶性膳食纤维的最适工艺参数,以液固比、温度、时间和碱浓度为试验因子,以可溶性膳食纤维产率为响应值,采用中心旋转组合试验设计进行试验。结果表明：4个因素对可溶性膳食纤维产率的影响大小依次为碱浓度＞液固比＞温度＞时间。通过典型性分析得出可溶性膳食纤维最适制备条件为：液固比26∶1、温度89℃、时间68 min、碱浓度1.12%。在此条件下,可溶性膳食纤维产率的预测值为33.96%,验证试验所得可溶性膳食纤维产率为34.12%。回归方程的预测值和试验值差异不显著,所得回归模型拟合情况良好,达到设计要求。在本试验优化的条件下,以经挤压豆渣为原料制备的可溶性膳食纤维产率（34.12%）显著高于以未经挤压豆渣为原料的产率（13.51%）。     

漆酶不同施用方法对土壤DDT污染修复的研究

该文从投加量、分次投加和灭菌等方面,研究了漆酶不同施用方法对其修复土壤DDT污染效果的影响.研究结果表明,土壤中DDT各组分(P,P'-DDE除外)及DDT总量(DDTs)的降解率均随着漆酶投加量的增加而显著提高,在投加量为每克土加酶6U时DDTs的降解率达到50.63%:漆酶两次投加对土壤中DDT各组分及总量的降解率均显著高于一次投加,DDTs的降解率提高11.4%;漆酶处理对于非灭菌土壤和灭菌土壤中DDT总量的降解率几乎相当,但各组分则有显著差异,其中P,P'-DDE、O,P'-DDT和P,P'-DDD在非灭菌土壤中的降解率低于灭菌土壤,而P,P'-DDT则相反.     

Residue depletion study and withdrawal period for flunixin-N-methyl glucamine in bovine milk following intravenous administration

The objective of this study was to establish a withdrawal period for flunixin in milk by quantifying 5-hydroxyflunixin, the marker residue, in bovine milk as a function of time, following intravenous treatment of lactating dairy cows with flunixin-N-methyl glucamine (Banamine or Finadyne). Lactating dairy cows were dosed on three consecutive days at 2.2 mg of flunixin free acid/kg of body weight/day. Milk was collected twice daily and assayed using a liquid chromatography-mass spectrometry/mass spectrometry (LC-MS/MS) procedure. The method was validated at concentrations in the range 0.5-250 ppb. The concentrations for 5-hydroxyflunixin measured 12 h after the last administration of drug ranged from 1.56 to 40.6 ppb for all cows. Milk concentrations for 5-hydroxyflunixin were used to establish withdrawal periods of 36 h using guidelines established by the U.S. Food and Drug Administration/Center for Veterinary Medicine and 24 h using guidelines established by the European Medicinal Evaluation Agency/Committee on Veterinary Medicinal Products.     

小麦和土壤中环丙唑醇残留消解动态及膳食摄入评估

为评价环丙唑醇在小麦生产上应用的安全性,通过建立乙腈提取、氮磷检测器检测方法对小麦籽粒、植株和土壤样品中环丙唑醇的残留量进行检测,研究了小麦籽粒、植株和土壤中环丙唑醇的残留及其消解动态,并对小麦中的残留量进行风险评估。结果表明,环丙唑醇在小麦籽粒、植株及土壤空白样品中的添加回收率为79.2%~95.6%,相对标准偏差为1.9%~10.0%,最小检出量为8.2×10?12 g,在小麦籽粒、植株及土壤中的最低检测浓度均为0.05 mg·kg?1,乙腈提取、氮磷检测器检测方法重现性好,准确度、精密度高,可满足环丙唑醇在小麦上的残留分析要求。2010年和2011年,河南省、黑龙江省和江苏省3地环丙唑醇在小麦植株和土壤中的消解半衰期分别为3.0~5.5 d、18.1~34.5 d;不同施药次数、施药量及采样间隔,环丙唑醇在小麦籽粒中的最终残留量均≤0.415 mg·kg?1。采收间隔期为14 d和21 d时,不同施药次数、施药剂量和采收间隔期,环丙唑醇在小麦植株、小麦籽粒和土壤中的残留量差异均不显著;采收间隔期为7 d,有效成分108 g?hm-2施药2次与有效成分162 g?hm-2施药3次时小麦植株、小麦籽粒和土壤中的残留量之间均存在显著性差异。普通人群环丙唑醇的国家估算每日摄入量为0.000 109 9 mg,占日允许摄入量的0.5%左右,按本试验方式进行施药,通常不会对一般人群健康产生不可接受的风险。     

Desorption of DDT from a Contaminated Soil using Cosolvent and Surfactant Washing in Batch Experiments

1,1-bis(p-chlorophenyl)-2,2,2-trichloroethane (p,p′-DDT) is a recalcitrant organic compound that is difficult to remove from contaminated soil due to its low solubility. In this study we investigated the effectiveness of both cosolvents and surfactants in enhancing the solubility of p,p′-DDT from a soil that has been contaminated with DDT for nearly 40 yr. The presence of selected surfactants removed less than 1 to 11% of p,p′-DDT compared to cosolvents, which removed less than 1 to 77% of p,p′-DDT from the same soil. The low solubility of p,p′-DDT in the presence of surfactants was attributed to the decreased surfactant concentration to below critical micelle concentrationfollowing sorption by soil surfaces. Enhanced solubility of p,p′-DDT was achieved with the use of cosolvents that releasedup to 77% of p,p′-DDT from a contaminated soil. Increasing the solution concentration and hydrophobicity of the cosolvent increased the amount of p,p′-DDT desorbed. For example, the amount of p,p′-DDT desorbed increased in the order 5% 1-propanol << 50% ethanol << 50% 1-propanol. Repeated washing of the soil with various cosolvents, in all but two cases, markedly increased the total amount of p,p′-DDT desorbed from the soil. For example, repeated washing of the soil with 50% ethanol increased the amount of p,p′-DDT removed by 42% while repeated washings of the soil with 50% 1-propanol had little effect on the amount of p,p′-DDT desorbed. Increasing the soil-solution ratio from 1:2 to 1:10 in the presence of 40% 1-propanol increased the amount of p,p′-DDT desorbed by 100%; suggesting that the soil-solution ratio was an important parameterin controlling the amount of p,p′-DDT desorbed.     

Tissue residues and urinary excretion of zilpaterol in sheep treated for 10 days with dietary zilpaterol

Zilpaterol is a beta-adrenergic growth promoter approved in Mexico and South Africa for use in cattle. Understanding the rates of zilpaterol depletion from tissues and urine is of interest for the development of strategies to detect the off-label use of zilpaterol. Eight sheep were fed 0.15 mg/kg/day dietary zilpaterol hydrochloride (Zilmax) for 10 consecutive days; two sheep each were slaughtered 0, 2, 5, and 9 days after discontinuation of exposure to the zilpaterol-containing diet. Tissue zilpaterol levels rapidly decreased during the withdrawal period. On the basis of LC-MS/MS-ES (external standard) measurements, liver zilpaterol residues in sheep were 29.3, 1.5, 0.13, and 0.10 ng/g after 0, 2, 5, and 9 day withdrawal periods, respectively; kidney residues were 29.6, 1.10, and 0.09 ng/g and below the detection limit; and muscle residues were 13.3, 0.86, 0.12, and 0.08 ng/g at the same respective withdrawal periods. Between-animal variation in urinary zilpaterol concentrations during the feeding period was considerable, although zilpaterol concentrations converged somewhat as steady state was reached. During the first 3 days of the withdrawal period, zilpaterol elimination followed a first-order excretion pattern, having an average elimination half-life of 15.3 +/- 1.8 h. Urinary zilpaterol concentrations during the withdrawal period were determined using ELISA, HPLC-fluorescence, LC-MS/MS-ES (external standard), and LC-MS/MS-IS (internal standard). Comparison of these methods showed a high correlation with each other. With the exception of LC-MS/MS-IS, the regression coefficients of the linear equations with a zero intercept were between 0.90 and 1.25, indicating the near equivalence of the methods. Because of its simplicity, ELISA is a convenient assay for determining zilpaterol levels in urine giving similar results to HPLC-fluorescence and LC-MS/MS-ES without requiring the extensive cleanup of the latter methods.     

Antimicrobial residue detection in chicken yolk samples following administration to egg-producing chickens and effects of residue detection on competitive exclusion culture (PREEMPT) establishment

Competitive exclusion (CE) cultures may offer alternatives to antimicrobial agents for disease prophylaxis in poultry. To avoid potential transfer of antibiotic resistance, safe and effective CE cultures must, by necessity, be highly sensitive to antimicrobial residues. The following studies evaluated the effect of maternal administration of selected antibiotics on the establishment of a licensed CE culture, PREEMPT. Selected antibiotics were administered to actively laying hens for a period of 7 days (experiment 1) or 9 days (experiment 2) in drinking water [sulfadimethoxine (0.05%), enrofloxacin (0.005%), and tylosin tartrate (0.05%)] or feed (sulfadimethoxine with ormetoprim, 250 ppm). In experiment 1, fertile eggs were collected daily and subjected to bioassay for detectable antimicrobial residues in yolk. Antimicrobial residues were not detected during the 7 days of treatment or the subsequent 3 days following cessation of treatment in the control, sulfadimethoxine, sulfadimethoxine with ormetoprim, or tylosin treatment groups. However, detectable residues were observed in eggs derived from enrofloxacin-treated hens on days 6 and 7 during antibiotic administration and also on days 2 and 3 post-antibiotic administration. In experiment 2, antimicrobial residues were also only detected in yolks from hens treated with enrofloxacin. Residue detection occurred on days 2-6 of antibiotic administration, on day 9 of antibiotic administration, on days 1-3 post-antibiotic administration, and also on day 7 post-antibiotic administration. A subset of eggs from each experimental group, corresponding to days 2-6 of antibiotic administration, days 4-6 post-antibiotic administration, and days 14-16 post-antibiotic administration, were pooled for incubation, and chicks hatched from these pools of fertile eggs were treated with PREEMPT at hatch. When 48-h cecal propionate concentrations were used as an index of culture establishment, reduced (P < 0.05) efficacy was observed only in chicks derived from enrofloxacin-treated hens at either collection period. Although several antibiotics do not appear to produce detectable egg residues or interfere with CE culture establishment, these data suggest that chicks derived from enrofloxacin-treated hens may not be candidates for safe and effective CE culture treatment.