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1.
Nitrofurans were broadly used as an extremely effective veterinary antibiotic especially in pig and poultry production farms. Because of fears of the carcinogenic effects on humans, the nitrofurans were banned from use in livestock production in many countries, including the European Union. The present study examines the accumulation, distribution, and depletion of furaltadone and nifursol and of their tissue-bound metabolites [3-amino-5-morpholinomethyl-2-oxazolidinone (AMOZ) and 3,5-dinitro-salicylic acid hydrazine (DNSAH), respectively, in poultry edible tissues (muscle, liver, and gizzards) following administration to chickens of therapeutic and subtherapeutic concentrations of both compounds. Nitrofurans determination was performed by high-performance liquid chromatography-diode array detection and liquid chromatography-tandem mass spectrometry, respectively, for feeds and for poultry tissues. Furaltadone and nifursol, in very low concentrations, were found in samples of muscle, liver, and chicken's gizzard collected from slaughtered animals after 5 weeks of treatment and no withdrawal time period. When a withdrawal time period of 3 weeks was respected, no detectable nitrofuran parent compounds was observed in all of the studied matrices. For AMOZ, concentrations of 270 μg/kg in meat, 80 μg/kg in liver, and 331 μg/kg in gizzard were determined after administration of a medicated feed with furaltadone (132 mg/kg), 3 weeks after withdrawal of treatment. For DNSAH, the concentration values obtained are much lower than those observed for AMOZ. For meat, liver, and gizzard, DNSAH concentrations of 2.5, 6.4, and 10.3 μg/kg, respectively, were determined, after administration of a medicated feed with nifursol (98 mg/kg), 3 weeks after withdrawal of treatment. The gizzard could be considered a selected matrix for nitrofuran residues evaluation in poultry, due to its capacity of retaining either nitrofuran parent compounds or metabolites in higher concentrations, regardless of the administered dose or of the respected withdrawal time period.  相似文献   

2.
珠江三角洲典型地区表层农田土壤中多氯联苯残留状况   总被引：7，自引：2，他引：5  
采集了珠江三角洲典型区域384个表层农田土壤样品,分析了其中常见6种土壤多氯联苯(PCB28、PCB52、PCB101、PCB138、PCB 153与PCB180)的残留状况.研究结果表明:6种多氯联苯总量(Σ6PCBs)的检出率为78.13％,其平均值为0.42 μg/kg. PCB138的检出率与含量高于其他5种PCBs;土壤中6种多氯联苯的残留状况存在很大的差异;PCB101的检出率最低,仅为10.16％,但其平均值(0.11 μg/kg)较高,主要源于某点位PCB101高达32.44 μg/kg,土壤受到了严重污染.线性相关关系分析结果表明:土壤有机质、黏粒含量则与PCB52存在显著正相关关系.总体而言,低氯代的PCBs含量与土壤理化性质具有一定的相关性,高氯代的PCBs呈现典型的点位污染且在点位土壤中其含量显著高于低氯代同系物.  相似文献   

3.
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.  相似文献   

4.
The occurrence of perchlorate in soybean sprouts (Glycine max L. Merr), water dropwort (Oenanthe stolonifera DC.), and lotus (Nelumbo nucifera Gaertn.) root, which are commonly consumed by people in South Korea, was determined by using an ion chromatograph coupled with a tandem mass spectrometer. For soybean sprouts (11 samples), perchlorate was detected in most (91%) of the samples at various concentrations of up to 78.4 μg/kg dry weight (DW); the mean concentration was 35.2 μg/kg DW. For water dropwort, of the 13 samples examined, four showed concentrations that were above the limit of quantification (LOQ). The mean perchlorate concentration was 20.7 μg/kg DW, and the highest perchlorate value was 39.9 μg/kg DW. Of the six lotus root samples examined, only one exhibited a detectable perchlorate concentration (17.3 μg/kg DW). For the accumulation experiments with artificially contaminated solutions, the concentrations of perchlorate in soybean sprouts gradually increased with the increase of perchlorate concentration in the solution. However, there was a decrease in the bioconcentration factor as the perchlorate concentration in the solution increased.  相似文献   

5.
A new method has been developed and validated for the simultaneous determination of four biogenic (putrescine, cadaverine, histamine, and tyramine) and three volatile amines (trimethylamine, triethylamine, and tripropylamine) in anchovy. Separation and determination of the selected compounds were carried out by ultra-high-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS), using an electrospray ionization source (ESI) in positive ion mode. Chromatographic separation was carried out using an aqueous solution of formic acid (0.1%) and methanol as mobile phase in gradient mode. The method was validated, and mean recoveries were evaluated at three concentration levels (75, 150, and 250 μg/kg), ranging from 70 to 110% at the three levels assayed. Intra- and interday precision, expressed as relative standard deviation (RSD), were lower than 15% and 20%, respectively. Limits of quantitation (LOQs) were 25 μg/kg for all cases, except for that of TMA, which was set at 60 μg/kg. The developed procedure was applied to determine the target compounds in anchovy samples stored during 7 days at 4 °C, observing the increasing in the concentration of these compounds at longer storage time.  相似文献   

6.
Twenty-six veal calves were split into two groups and fed two milk replacers with a different content of phytosterols for 26 days; then, 14 calves (7 animals from each diet) were kept as controls and 12 calves (6 per diet) received daily, per os, a combination of 17beta-boldenone (17beta-Bol) and androsta-1,4-dien-3,17-dione (ADD) for 38 days. The urinary elimination of 17 alpha-/17beta-boldenone conjugates (17 alpha/beta-Bol) and androsta-1,4-dien-3,17-dione (ADD) was followed by liquid chromatography-tandem mass spectrometry from all of the animals until slaughtering. In urine from treated animals, 17 alpha-Bol concentrations, despite a great variability, were greater than 17beta-Bol, both detected always as conjugates. At days 1, 2, and 3, the mean urine concentration of 17 alpha-Bol was higher than 12 ng/mL. A remarkable decrease was observed during the following days, but the 17 alpha-Bol concentration was still higher than the attention level of 2 ng/mL in 58% of the samples; the concentration of 17beta-Bol was around the action level of 1 ng/mL; two days after treatment withdrawal, no 17beta-Bol was detected in the urine. In urine from control animals, the 17 alpha-Bol concentration was strictly related to the phytosterol content of the diet, while, in urine from treated animals, the much higher 17 alpha-Bol levels were not modified by the production from diet precursors. The results confirmed that a 17 alpha-Bol level higher than 2 ng/mL should be considered as evidence of suspected illegal treatment and that the urinary excretion of 17beta-Bol is due to exogenous administration of 17beta-Bol. The discontinuous rate of elimination of both 17 alpha- and 17beta-Bol, despite the daily administration of 17beta-Bol plus ADD, indicates the necessity for further research to detect other urinary boldenone metabolites to strength surveillance strategy.  相似文献   

7.
The use of nitrofurans as veterinary drugs has been banned from intensive animal production in the European Union (EU) since 1993. The objective of the present study was to evaluate the accumulation and depletion of furaltadone and nifursol and their side-chain metabolites 5-methylmorpholino-3-amino-2-oxazolidinone (AMOZ) and 3,5-dinitrosalicylic acid hydrazide (DNSAH) in eggs after administration of therapeutic and subtherapeutic doses of the drugs to laying hens during three consecutive weeks. LC-MS/MS, with positive and negative electrospray ionization methods, was used for the determination of parent compounds and metabolites in yolk and egg white and was validated according to criteria established by Commission Decision 2002/657/EC. The decision limit (CCα) and the detection capability (CCβ) of the analytical methodology for metabolites were 0.1 and 0.5 μg/kg for AMOZ and 0.3 and 0.9 μg/kg for DNSAH, respectively. For the parent compounds, CCα and CCβ were 0.9 and 2.0 μg/kg for furaltadone and 1.3 and 3.1 μg/kg for nifursol, respectively. The data obtained show that the parent compounds are much less persistent than their side-chain metabolites in either yolk or egg white. Between the studied metabolites, AMOZ is the most persistent and could be detected in either yolk or egg white three weeks following withdrawal from treatment.  相似文献   

8.
An on-line solid-phase extraction (SPE) following a liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) method was established for the simultaneous analysis of bisphenol A (BPA), nonylphenol (NP), and octylphenol (OP) in cereals (including rice, maize, and wheat). The target compounds were extracted by acetonitrile, purified by an automated on-line SPE cartridge, and analyzed by LC-MS/MS under the negative-ion mode. Mean recoveries fortified at three concentration levels ranged from 81.6 to 115.7%, and the coefficient of variation ranged from 4.6 to 19.9% (n = 6). The limits of quantification (LOQs) of the method were 0.5, 0.5, and 0.25 μg/kg for BPA, NP, and OP, respectively, in both rice and maize, while the LOQs in wheat were 0.5, 1.25, and 0.5 μg/kg for BPA, NP, and OP, respectively. This method was applied in the analysis of rice, maize, and wheat from a local market. As a result, NP occurred in all cereal samples at the concentration range of 9.4-1683.6 μg/kg and BPA was detected in a few samples.  相似文献   

9.
The distribution of oxytetracycline (OTC) in male and female Macrobrachium rosenbergii was examined after the prawns had been given medicated feed containing OTC at levels of 2.5 and 5.0 g/kg of feed for 1 week and nonmedicated feed thereafter. OTC levels in the heads of both male and female prawns were consistently higher than in the muscles. Batches of both male and female prawns treated with higher dosages had significantly higher OTC residues in both head and muscle tissues than the batches treated with lower dosages. During treatment, peak concentrations in the head and muscle from each group were reached within 4-6 days. After drug treatment ceased, 13 days for the head and 10 days for the muscle were required to reduce OTC residues to safe levels in all batches of both sexes and dosages. In practice, to account for variations in water temperature, drug dosage, duration of therapy, and other environmental conditions, a withdrawal period of 21 days is recommended.  相似文献   

10.
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.  相似文献   

11.
天然富硒土壤上三种蔬菜对硒的吸收与转化差异   总被引：1，自引：1，他引：0  
【目的】研究对硒 (Se) 不同敏感性蔬菜对天然富硒土 (Se ≥ 0.4 mg/kg) 中硒的吸收和转化差异,为富硒土壤生产富硒蔬菜提供理论与技术指导。【方法】以大蒜、芥菜和菠菜三种蔬菜为试验材料,在全硒含量为0.29、0.58、0.98、2.07 mg/kg的四种土壤上进行了盆栽试验 (依次标记为Se0.29、Se0.58、Se0.98、Se2.07),并测定四种土壤中不同形态硒的含量。芥菜和菠菜于生长40 d、53 d、68 d和82 d后取样,测定蔬菜可食部分硒含量;于生长97 d后收获,分为根部和地上部。大蒜于生长42 d、68 d、82 d、120 d后取样,测定地上部硒含量;于生长165 d后收获,分为根部、鳞茎和叶。测定供试蔬菜总硒含量、有机硒含量,计算不同硒含量土壤上蔬菜对硒的吸收和转化系数。【结果】三种蔬菜中芥菜的生长对土壤硒最为敏感,芥菜可食部位生物量鲜重以Se0.29处理最高,菠菜和大蒜均以Se0.58处理最高,与Se2.07处理均达显著差异。三种蔬菜地上部硒含量在整个生育期总体呈现增加的趋势,不同生育期均表现为大蒜 > 芥菜 > 菠菜。收获期三种蔬菜各部位的硒含量随着土壤硒含量 (0.29～2.07 mg/kg) 的增加而增加,表现为Se2.07 > Se0.98 > Se0.58 > Se0.29,Se2.07处理的菠菜地上部和地下部硒含量分别是其Se0.29处理的8.63倍和7.10倍,芥菜是12.25倍和23.29倍,Se2.07处理大蒜鳞茎和叶部硒含量是Se0.29处理的39.92倍和4.90倍;可食部位硒含量为大蒜 (7.25～289 μg/kg) > 芥菜 (1.22～14.9 μg/kg) > 菠菜 (0.73～6.30 μg/kg),均表现为地下部 > 地上部,Se2.07处理菠菜根部硒含量是茎叶的4.80倍,芥菜是12.06倍,大蒜是8.22倍。在富硒土壤Se0.98和Se2.07处理条件下,大蒜和芥菜能从土壤中富集硒,吸收系数是菠菜的3.06～8.47倍和1.58～5.8倍,均达到了富硒蔬菜标准 (≥ 0.01 mg/kg)。三种蔬菜可食部位有机硒含量占总硒比例为73.5%～84.7%,并随土壤硒含量的增加而增加,其中Se2.07与Se0.29处理差异显著;蔬菜硒含量不但与土壤总硒含量相关,而且与有效态硒含量呈显著正相关。【结论】蔬菜种类和土壤硒含量均影响蔬菜硒的吸收、转化和富集。三种蔬菜对土壤硒的敏感性以芥菜最强。蔬菜硒含量和可食用部位有机硒的转化率均随着土壤硒含量的增加而增加,与土壤总硒含量和有效态硒含量呈显著正相关。富硒能力为大蒜 > 芥菜 > 菠菜,在天然富硒土壤上生长的大蒜和芥菜硒含量易达到富硒蔬菜标准,而菠菜未显示出富硒能力。因此,虽然土壤硒含量高影响了大蒜和芥菜的生长,但大蒜和芥菜具有较强的将硒转移到可食部位的能力,可作为富硒蔬菜生产。  相似文献   

12.
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.  相似文献   

13.
采用现场采样及室内测试方法对广州某氮肥厂原料车间和油库区土壤中16种优控多环芳烃（PAHs）的含量进行调查研究,分析了EPAHs含量及其组成特征和垂直分布特征,并在此基础上进行了源解析。结果表明,分析样品中∑PAHs范围在10-7795μg·kg,原料车间土壤中的∑PAHs小于油库区土壤中的,菲、芘、荧蒽、并（b）荧蒽、苯并（a）芘为主要污染物;油库土壤0-40cm的样品中16种PAHs均有检出,∑PAHs和单体分布基本一致;原料车间土壤∑PAHs和单体浓度随着地面深度的增加而减少。通过对单组分比值（菲／蒽,荧蒽／芘）的分析可以看出油库区土壤中PAHs来源于石油和燃烧源,而原料车间污染源主要为燃烧源。  相似文献   

14.
A reliable analytical method was presented for the simultaneous determination of six N-nitrosamines, nine aromatic amines, and melamine in milk and dairy products using gas chromatography coupled with mass spectrometry. The sample treatment includes the precipitation of proteins with acetonitrile, centrifugation, solvent changeover by evaporation, and continuous solid-phase extraction for cleanup and preconcentration purposes. Samples (5 g) containing 0.15-500 ng of each amine were analyzed, and low detection limits (15-130 ng/kg) were achieved. Recoveries for milk and dairy products samples spiked with 1, 10, and 50 μg/kg ranged from 92% to 101%, with intraday and interday relative standard deviation values below 7.5%. The method was successfully applied to determine amine residues in several milk types (human breast, cow, and goat) and dairy products.  相似文献   

15.
A novel multiresidue analysis method is developed for the determination of twenty phthalate esters at the μg/kg level in edible vegetable oils by microwave-assisted extraction-gel permeation chromatography-solid phase extraction-high resolution gas chromatography-tandem mass spectrometry (MAE-GPC-SPE-HRGC-MS/MS). The samples were extracted with methanol under microwave incubation. Cleanup was carried out with GPC followed by a further C18 SPE column and then separated by the HP-5MS capillary column under a temperature program. The eluents were qualitatively and quantitatively determined by tandem mass analyzer with selected reaction monitoring (SRM) type and positive ion mode. The calibration curves showed good linearity in the range 5 μg/kg to 2.50 mg/kg with correlation coefficients larger than 0.999. Low detection limits (LODs) of 0.218-1.367 μg/kg and quantification limits (LOQ) of 0.72-4.51 μg/kg were achieved. The mean recoveries were in the range from 93.04% to 104.6% at 5, 15, and 40 μg/kg spiked levels, and the relative standard deviations (RSDs) were in the range of 1.01% and 5.26% (n = 7). This method could potentially overcome the interference from large amounts of lipids and pigment. The real sample test showed this method can be used for sensitive and accurate determination and confirmation of phthalate ester residues in high-fat and complex samples.  相似文献   

16.
应用RIA测定奶中孕酮含量诊断奶牛卵巢机能性疾病   总被引：1，自引：1，他引：1  
吴美文 《核农学报》1988,2(1):55-60
正常奶牛一个发情周期由卵泡期、黄体期、黄体生长期和黄体消解期所组成。根据30头正常奶牛的临床观察和测定各个时期的奶中孕酮含量表明,卵泡期奶中孕酮含量为≤5ng/ml,持续时间为4.5±1.5天;黄体期奶中孕酮含量为≥11ng/ml,持续时间为13±2天;黄体生长期奶中孕酮含量为>5ng/ml—<11ng/ml,持续时间为2±1天;黄体消解期奶中孕酮含量为<11ng/ml—75ng/ml,持续时间为1±0.5天.根据这些指标并结合奶牛的临床表现对奶牛的卵巢机能性疾病进行了诊断,获得了较好的结果,提高了诊断的准确率。  相似文献   

17.
Depletion of moxidectin tissue residues in sheep   总被引：1，自引：0，他引：1  
The pattern of tissue depletion of moxidectin (MXD) subcutaneously administered to sheep was characterized in this study. MXD concentration profiles were determined in muscle, fat, and liver and at the site of injection following administration of a formulation combining MXD (0.5% w/v) with a standard 6 in 1 clostridial vaccine. Thirty-five (35) parasite-free Lincoln sheep were treated with the MXD injectable formulation at a dose rate of 0.2 mg of MXD/kg of live weight, administered subcutaneously on the inner surface of the thigh. Treated animals were sacrificed in randomly selected groups of six sheep weekly from day 21 until day 49 post-treatment. Three nontreated animals were sacrificed to obtain blank tissue samples to validate the analytical methodology. MXD concentration profiles were determined by a validated HPLC analytical method using fluorescence detection. MXD has an adequate pattern of absorption, based on the low residual concentrations found in the injection site area at all sampling intervals. Muscle samples showed the lowest MXD concentrations throughout the study period. The highest MXD concentrations at all sampling times were measured in the adipose tissue, indicating that fat is a target tissue for MXD. MXD concentrations in all of the tissues analyzed were below the accepted maximum limit of residue at 21 days post-treatment.  相似文献   

18.
A dioxin-contaminated mineral supplement was used to study the bioaccumulation and elimination of dioxins in two dairy cows. The supplement was mixed into the total maintenance ration and fed to the cows for 40 days after which unfortified diets were fed for 40 additional days. Dioxins and coplanar polychlorinated biphenyls (PCBs) were measured twice a week in the milk and in selected tissues of the cows, one at death (day 10 of withdrawal) and one at slaughter (day 40 of withdrawal). The dioxins and PCBs were readily transferred into the milk, and at steady state, total toxic equivalents were concentrated 6-fold into the milk fat from the diet. Bioaccumulation was inversely related to chlorination number. The elimination of dioxins and PCBs in milk was biphasic. With the exception of 1,2,3,4,6,7,8-heptachlorodioxin and both octachlorinated congeners, dioxin and furan half-lives in milk were approximately 3-5 days for the alpha-phase and 35-50 days for the beta-phase. PCB-169 had a longer half-life: 11 (alpha) and 200 days (beta). When milk and feed samples from Minnesota farms that had used similar contaminated mineral supplements were analyzed, no elevated dioxin levels were found in milk. It appeared that although the dioxins from the mineral supplements have the potential to bioaccumulate, dilution into the total diet was sufficient to prevent a significant rise in the dioxin concentrations in the milk at these farms.  相似文献   

19.
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.  相似文献   

20.
盆栽试验研究了不同磷肥水平下接种丛枝菌根菌（Arbuscular mycorrizal fungi,AMF）对玉米修复芘污染土壤的影响。结果表明,在施磷水平为20和80 mg/kg条件下,50 mg/kg芘处理土壤中丛枝菌根菌能够正常侵染玉米根系,侵染率没有显著变化;土壤芘污染对玉米的生长有抑制作用,缺磷土壤中施磷能够缓解土壤芘对玉米生长的抑制作用。培养60 d后,高磷（80 mg/kg）和低磷（20 mg/kg）条件下,玉米接种AMF处理土壤芘残留浓度分别比相应的不接种处理降低了38%和35%,比相应无玉米的对照处理降低了53%和58%。表明玉米接种混合AMF能够显著降低土壤芘残留浓度,促进土壤芘的去除。与P 20 mg/kg处理相比,P 80 mg/kg处理玉米接种及不接种AMF的土壤芘残留浓度分别降低了16%和19%,表明缺磷土壤中施磷对玉米及菌根玉米去除土壤芘均有一定促进作用。土壤微生物碳量与土壤芘的去除率显著正相关,接种AMF和P 80 mg/kg处理均能够显著增加土壤微生物碳量,因此土壤微生物数量的增加可能是其促进土壤芘的去除的重要原因。  相似文献   

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