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1.
经丙酮、二氯甲烷提取,饱和正己烷脱脂,氮吹仪吹干浓缩后,以乙腈-磷酸二氢钠溶液(0.01 mol/L,含0.005mol/L十二烷基硫酸钠和0.1%三乙胺)(35 :65)为流动相,流速为1.0 mL/min,荧光检测激发波长为225 nm,发射波长285 nm.氟苯尼考在0.01～10.0 mg/L、氟苯尼考胺在0.002 5～2.5 mg/L浓度范围内,本方法线性关系良好,相关系数分别为0.999 7和0.999 8.当添加水平氟苯尼考为15～500 μg/kg、氟苯尼考胺为5～500μg/kg时.该方法平均回收率分别为79.5%～84.6%和80.7 0A～88.2%,相对标准偏差分别为2.8%～6.4%和2.4%～5.3%;检测限分别为5μg/kg和μg/kg.该方法样品处理简单,可同时检测氟苯尼考和氟苯尼考胺的残留,且准确度和精密度均符合残留分析的要求. 相似文献
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虾肌肉中氟苯尼考和氟苯尼考胺残留的高效液相色谱检测方法研究 总被引：1，自引：1，他引：0
[摘 要] 建立了虾肌肉中氟苯尼考和氟苯尼考胺残留的高效液相色谱检测法。以水和丙酮为提取溶液,Oasis MCX固相萃取柱净化,采用Inertsil ODS-3(5μm , 250mm×4.6mm i.d.)反相色谱柱,以比例为68:32的A液（0.02 mol/L戊烷磺酸钠—0.025 mol/L磷酸钠溶液,pH 3.85）与B液（含0.1%三乙胺的甲醇溶液）为流动相,在225nm处检测。氟苯尼考和氟苯尼考胺在10～1000 µg/kg浓度范围内,线性关系良好;添加浓度为50、100、200、500 μg/kg时,回收率在75.8%～85.9%,日内变异系数在 2.4%～4.5%,日间变异系数在 4.0%～5.8%;方法的检测限为10 μg/kg,定量限为30 μg/kg。本方法灵敏、准确、简便、快速,适于虾肌肉中氟苯尼考和氟苯尼考胺残留的同时检测。 相似文献
3.
氟苯尼考及其代谢物氟苯尼考胺在鸡肌肉中的残留消除规律 总被引：1，自引：0，他引：1
本试验旨在研究氟苯尼考及其代谢物氟苯尼考胺在鸡肌肉中的残留消除规律。鸡肌肉样品经丙酮、二氯甲烷提取,饱和正己烷脱脂,氮吹仪吹干浓缩后,以乙腈-磷酸二氢钠溶液(0.01mol.L-1,含0.005mol.L-1十二烷基硫酸钠和0.1%三乙胺)(体积比35∶65)为流动相,流速为1.0mL.min-1,在激发波长225nm、发射波长285nm处用高效液相色谱荧光检测器检测。结果:测得鸡肌肉中氟苯尼考、氟苯尼考胺的检测限分别为1.5和0.5μg.kg-1(S/N=3)、定量限分别为5和2μg.kg-1(S/N=10)。各试验组京海黄鸡分别按体质量以25.0、50.0和100.0mg.kg-1.d-1剂量给药,每天1次,连续5d内服给药后,休药第1天时,鸡肌肉中氟苯尼考及其代谢物氟苯尼考胺的残留量均达到峰值,且残留量随给药剂量的增大而增大,随休药期的延长而降低。休药第7天时,鸡肌肉中氟苯尼考及其代谢产物氟苯尼考胺的总残留量均低于MRLs(100μg.kg-1);休药第11天时,鸡肌肉中氟苯尼考及其代谢产物氟苯尼考胺的总残留量均低于检测限;氟苯尼考、氟苯尼考胺在鸡肌肉中的残留量及其总残留量均与给药剂量呈正相关。 相似文献
4.
建立了土壤中氟苯尼考及氟苯尼考胺高效液相色谱(HPLC)检测方法。土壤样品采用超声提取法,提取试剂为丙酮和水,再与二氯甲烷进行液-液萃取净化杂质。Agilent SB-C18色谱柱进行分离后,光电二极管阵列检测器检测,流动相为磷酸二氢钠溶液(0.01 mol/L,含0.005 mol/L十二烷基硫酸钠,pH=4.4)和乙腈(V∶V=65∶35)。在0.025～5 mg/L浓度范围内,峰面积与浓度呈良好的线性关系,相关系数r均达0.999,氟苯尼考及氟苯尼考胺检测限分别为0.01、0.015 mg/kg,定量限分别为0.045、0.05 mg/kg。三种土壤中添加浓度为0.05、0.1、0.2 mg/kg时,氟苯尼考和氟苯尼考胺标准工作液的回收率分别为90.16%～99.37%、67.63%～96.86%,日内变异系数均≤7.83%,日间变异系数均≤10.52%。该方法高效快速,操作简单,成本低,可用于氟苯尼考及氟苯尼考胺的同时检测。 相似文献
5.
水产品中甲砜霉素、氟苯尼考和氟苯尼考胺酶联免疫多残留测定 总被引：6，自引：2，他引：4
将氟苯尼考胺与载体蛋白相连作为抗原免疫动物,获得抗甲砜霉素等药物的抗体,建立了水产品中甲砜霉素、氟苯尼考和氟苯尼考胺残留的ELISA检测方法。结果显示,人工抗原中氟苯尼考胺与蛋白质分子的结合比约为12∶1,血清效价达到1∶2000倍以上,50%抑制浓度(IC50)为3μg/L左右,3种酰胺醇类药物交叉反应率在30%～156%之间,鱼和虾肌肉组织中的检测限分别为6.3μg/kg和6.1μg/kg,在鱼和虾肌肉组织中三种药物的回收率在40%～120%之间,检测范围为0.2～125μg/L。该方法可同时测定甲砜霉素、氟苯尼考及其标示残留物氟苯尼考胺等3种化合物残留量。方法灵敏度、精密度和准确度均能满足兽药残留筛选检测要求。 相似文献
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建立了超高效液相色谱串联质谱法检测禽蛋中氟苯尼考和氟苯尼考胺残留物的方法。采用电喷雾离子源（ESI）、多反应监测（MRM）、正负离子模式同时扫描检测,内标法定量。禽蛋试样采用碱化乙酸乙酯和乙腈提取,正己烷萃取,LC/MS-MS分析。结果表明,该方法的检测限（LODs）为0.1 μg/kg,定量限（LOQs）为0.2 μg/kg。在0.2~200 μg/L范围内均呈良好线性关系,并且3个添加浓度的平均回收率范围为70%~110%,相对标准偏差（RSD）小于10%。该方法简便高效、准确可靠,可作为禽蛋中氟苯尼考和氟苯尼考胺残留的检测方法。 相似文献
7.
研究三黄鸡摄入氟苯尼考一个月后,肝、肾、胸肌和油等组织中的残留消除规律.鸡组织经pH7.0的磷酸盐缓冲液和丙酮提取,经二氯甲烷萃取后氮吹仪上吹干、定容液定容,定容液经正己烷脱脂后过0.45μm滤膜,进液相色谱二极管阵列检测器.以乙腈-磷酸二氢钠(0.01mol/L,含5mmol/LSDS和体积分数为0.10%三乙胺)(体积比2:3)用磷酸调至4.5作流动相,用Sunfire C18柱(4.6×250mm,5μm),检测波长225nm.用该方法测定肝、肾、胸肌和油组织中环丙沙星的最低检测限为0.020mg/kg.三黄鸡分别用含氟苯尼考饲料连续喂养30d,记录休药后0d、1d、3d、5d、7d、9d,11d,14d,18d,32d时,肌肉、肾脏、肝脏组织中氟苯尼考和氟苯尼考胺残留量的变化.氟苯尼考和氟苯尼考胺在鸡的肝、肾、胸肌和油组织中残留量随着时间的延长而递减. 相似文献
8.
氟苯尼考粉中非法添加四种喹诺酮类药物的HPLC检测方法研究 总被引：1，自引：1，他引：0
建立了高效液相色谱法检测氟苯尼考粉中非法添加氧氟沙星、诺氟沙星、环丙沙星、恩诺沙星的方法.用十八烷基键合硅胶色谱柱,以A(磷酸3.0 mL加水至1000 mL,三乙胺调pH值至3.0±0.1,加乙腈50 mL)-甲醇(88:12)为流动相,采用二极管阵列检测器,采集波长为200 ～400nm,分辨率1.2 am,记录光谱图和283 nm波长处的色谱图,流速1.0 mL/min,柱温30℃.结果显示,4种喹诺酮类药物的浓度在0.5 ～ 200 μg/mL范围内呈良好的线性关系,添加回收率在98.5％ ～100.9％之间,相对标准偏差在0.14％ ～ 0.74％之间,检测限0.5 mg/g.本方法快速、准确,可用于氟苯尼考粉中非法添加喹诺酮类药物的定性和定量检测. 相似文献
9.
为监控鸡和猪组织中酰胺醇类药物残留,保障畜禽产品质量安全,建立了同时测定鸡和猪组织中甲砜霉素(TAP)、氟苯尼考(FF)及其代谢物氟苯尼考胺(FFA)残留量的气相色谱-质谱法(GC-MS)。样品经2%氨化乙酸乙酯溶液提取,PEP-2固相萃取柱净化,N,O-双三甲基硅烷三氟乙酰胺(BSTFA)衍生,气相色谱-质谱法测定,内标法定量。结果显示,甲砜霉素、氟苯尼考及其代谢物氟苯尼考胺在5～5000μg/L浓度范围内线性关系良好,相关系数r均大于0.999。本方法在鸡、猪肌肉、皮+脂(脂肪)、肝脏和肾脏中的检出限均为5μg/kg,定量限均为10μg/kg,在鸡和猪各空白组织添加10～5000μg/kg浓度水平下,其平均回收率在88.1%～106.4%之间,相对标准偏差在1.5%～10.8%之间。结果表明:本方法准确可靠,普遍适用于鸡和猪各组织中TAP、FF、FFA残留量的检测。 相似文献
10.
本研究通过高效液相色谱-串联质谱法(High Performance Liquid Chromatography-Tandem Mass Spectrometry,HPLC-MS/MS)建立了猪肉中氟苯尼考残留物残留量的检测方法,检测限和定量限分别为5μg/kg和10μg/kg。在10μg/kg~4000μg/kg浓度范围内,空白猪肉样品的标准曲线线性关系良好,相关系数均在0.99以上。氟苯尼考和氟苯尼考胺的添加浓度在10μg/kg、500μg/kg和2000μg/kg时,回收率均大于85%,批间和批内变异系数均小于5%。该方法适用于猪可食性组织中氟苯尼考残留量的测定。 相似文献
11.
Fan Yang Chao-Shuo Zhang Han Wang Fang Yang 《Journal of veterinary pharmacology and therapeutics》2020,43(1):79-86
The previously adopted marker residue for florfenicol (FF) in China was only florfenicol amine (FFA); however, the marker residue has been changed to FF plus FFA since the end of 2017. The previous official withdrawal period determined based on the only concentration of FFA may no longer be suitable. Therefore, the present study aimed to determine the depletion profiles of FF and FFA and further calculate the withdrawal period in the crucian carp (Carassius auratus) based on the new marker residues. Florfenicol was intramuscularly administered at 10 mg/kg bodyweight daily for five consecutive days to crucian carps reared in freshwater at 10°C. After the last dose, plasma and tissue samples were randomly collected from 10 fish at different time points. The FF and FFA concentrations were simultaneously determined by high-performance liquid chromatography (HPLC) with a fluorescence detector and further subjected to noncompartmental analysis. The elimination half-life (h) of FF in different tissues decreased as follows: liver (39.1) > kidney (36.3) > skin plus muscle (34.6) > plasma (31.7), whereas that of FFA decreased as follows: kidney (41.4) > skin plus muscle (39.4) > liver (39.3) > plasma (35.7). Considering a maximum residue limit of 1 μg/g for the total concentration of FF and FFA in the skin plus muscle, a withdrawal period of 6 days was calculated based on the upper limit of the one-sided 95% confidence interval. 相似文献
12.
A. Filazi U.T. Sireli B. Yurdakok F.G. Aydin A.G. Kucukosmanoglu 《British poultry science》2014,55(4):460-465
1. The aim of this study was to develop a suitable method for the analysis of florfenicol (FF) and its metabolite florfenicol amine (FFA) in chicken eggs and to determine FF and FFA residue depletion in eggs of laying hens.
2. The analytes were extracted from yolk, albumen and whole egg by phosphate buffer and ethyl acetate. Following purification, samples were analysed by high-performance liquid chromatography.
3. Fifty laying hens were divided into 5 groups, and each hen received doses of 20 mg/kg FF: Group 1 (received a single oral dose by gavage); Group 2 (a single intramuscular dose); Group 3 (a single subcutaneous dose); Group 4 (multiple oral doses for 3 d) and Group 5 (multiple oral doses for 5 d).
4. Limits of detection and of quantitation values were 1.94 and 6.45 g/109 g (ppb) for FF, respectively, and 0.48 and 1.58 ppb for FFA, respectively. Relative standard deviation values of intra-day and inter-day variation below 11% also confirmed the usefulness of the method for analysing FF and FFA in eggs.
5. From the first day of both oral and parenteral administration, FF and FFA were detected at 0.1% and 0.08% of dosage, respectively, and 57% of the drugs were eliminated from the egg yolk. Elimination time of FF was 8 d in Groups 1, 2 and 3; 9 d in Group 4 and 10 d in Group 5. 相似文献
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Pharmacokinetics of florfenicol and its metabolite florfenicol amine in crucian carp (Carassius auratus) at three temperatures after one single intramuscular injection 
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下载免费PDF全文 Fan Yang Fang Yang Tao Kong Guoyong Wang Dongying Bai Baobao Liu 《Journal of veterinary pharmacology and therapeutics》2018,41(5):739-745
The pharmacokinetic profiles of florfenicol (FF) or florfenicol amine (FFA) in crucian carp were compared at different water temperatures after single intramuscular administration of FF at 10 mg/kg bodyweight. The concentrations of FF and FFA were determined by a high‐performance liquid chromatography method, and then, the concentration versus time data were subjected to compartmental analysis using a one‐compartment open model. At the water temperatures of 10, 20, and 25°C, the peak concentrations (Cmaxs) of FF were 2.28, 2.29, and 2.34 μg/ml, respectively, while those of FFA were 0.42, 0.71, and 0.82 μg/ml, respectively. And the absorption half‐life (t1/2ka) of FF was 0.21, 0.19, and 0.21 hr, while the elimination half‐life (t1/2kel) was 31.66, 24.77, and 21.48 hr, respectively. For FFA, the formation half‐life (t1/2kf) was 3.85, 8.97, and 12.43 hr, while the t1/2kel was 58.34, 30.27, and 21.22 hr, respectively. The results presented here demonstrated that the water temperature had effects on the elimination of both FF and FFA and the formation of FFA. Based on the T > MIC values calculated here, to treat the infections of bacterial with MIC value ≤ 0.5 μg/ml, FF intramuscularly given at 10 mg/kg bodyweight with a 72‐hr interval is sufficient at the water temperature of 10°C, while the intervals of 60 and 48 hr were needed at 20 and 25°C, respectively. But to treat bacterial with higher MIC values, more FF or FF at 10 mg/kg BW but with shorter intervals should be intramuscularly given to the infected fish. 相似文献
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试验旨在比较洪江雪峰乌骨鸡和罗曼粉蛋鸡的鸡蛋营养成分和蛋品质,为洪江雪峰乌骨鸡蛋用新品系选育提供依据。随机选取40周龄的洪江雪峰乌骨鸡(绿壳)、洪江雪峰乌骨鸡(粉壳)和罗曼粉壳蛋鸡各100只,每品种鸡随机分为5个重复,每个重复20只,在相同饲粮和饲养管理方式下进行饲养,45周龄收集鸡蛋检测营养成分和蛋品质指标。结果表明:洪江雪峰乌骨鸡绿壳蛋的蛋黄比例极显著高于罗曼粉壳蛋(P<0.01),蛋重、蛋壳厚度、哈氏单位极显著低于罗曼粉壳蛋(P<0.01),洪江雪峰乌骨鸡粉壳蛋的蛋重和蛋壳厚度极显著低于罗曼粉壳蛋(P<0.01);洪江雪峰乌骨鸡蛋中的多不饱和脂肪酸和硒元素含量均极显著高于罗曼粉壳蛋(P<0.01),洪江雪峰乌骨鸡绿壳蛋胶原蛋白含量极显著高于罗曼粉壳蛋(P<0.01)。综上所述,洪江雪峰乌骨鸡鸡蛋蛋黄比例高,蛋黄多不饱和脂肪酸、胶原蛋白、硒和锰含量高,适合作为优质禽蛋开发。 相似文献
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Pharmacokinetics of veterinary drugs in laying hens and residues in eggs: a review of the literature
Poultry treated with pharmaceutical products can produce eggs contaminated with drug residues. Such residues could pose a risk to consumer health. The following is a review of the information available in the literature regarding drug pharmacokinetics in laying hens, and the deposition of drugs into eggs of poultry species, primarily chickens. The available data suggest that, when administered to laying hens, a wide variety of drugs leave detectable residues in eggs laid days to weeks after the cessation of treatment. 相似文献
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1. Anticoccidials are widely used as food additives to prevent and treat coccidiosis. They are licensed for use in a prescribed concentration and during a specific time interval with broilers and pullets, but not for laying hens. 2. This study was set up to develop a new high pressure liquid chromatography (HPLC) method to detect clazuril (CZ: (+/-)-2-chloro-alpha-(4-chlorophenyl)-4-(4,5-dihydro-3,5-dioxo-1,2,4-triazin-2(3H)-yl)-benzeneacetonitrile) in egg yolk and albumen and in plasma; to investigate both the presence of residues of CZ in eggs and its pharmacokinetic behaviour in laying hens. 3. A single oral dose (3 mg/kg BW) and multiple oral doses (3 mg/kg BW for 5 d) were investigated. The analytical method gave very good recovery (64 to 74%) in the three different matrices (yolk, albumen and plasma); precision and accuracy were within 11%. 4. After a single dose no residue was detected in eggs collected for up to 10 d, while following multiple dose treatment, CZ residues were detected until 10 d after the end of treatment. The concentration of the drug was higher in yolk than in albumen with a maximum ratio of 10 : 1. 5. Pharmacokinetics of CZ in laying hens after a single dose showed a detectable concentration of the drug up to 24 h. It reached a steady state after the third administration in multiple dosing. 6. Although further studies are necessary, these results indicate that a single oral dose of CZ could be used as an anticoccidial for laying hens due to the lack of residues in eggs. 相似文献