磺胺氯吡嗪钠—甲氧苄啶可溶性粉在鸡体内的残留消除研究

发布时间：2018-04-09 06:43

  本文选题：磺胺氯吡嗪钠-甲氧苄啶可溶性粉　切入点：鸡　出处：《扬州大学》2017年硕士论文

【摘要】：磺胺氯吡嗪钠-甲氧苄啶可溶性粉是一种复方新制剂,兽医临床上主要用于防控鸡球虫病。本实验通过建立鸡可食性组织(肌肉、肝脏、肾脏、皮脂)中残留标示物磺胺氯吡嗪(SPZ)和甲氧苄啶(TMP)残留量的HPLC检测方法,研究磺胺氯吡嗪钠-甲氧苄啶可溶性粉在鸡组织中的残留消除规律,为制订该复方新制剂在鸡的休药期提供理论依据。1.鸡可食性组织中磺胺氯吡嗪残留量的高效液相色谱检测方法鸡可食性组织样品中磺胺氯吡嗪残留采用氨水-乙腈(5/95,v/v)提取,正己烷除脂,MCX固相萃取小柱净化,高效液相色谱紫外检测器检测。流动相为乙腈-0.02 mol/L磷酸二氢钾水溶液(35/65,v/v),紫外检测波长为272 nm。外标法定量。结果显示,磺胺氯吡嗪标准溶液在0.08～20.00 μg/mL(0.04～10.00mg/kg)浓度范围内,呈良好的线性关系(r0.9999)。检测限(LOD)为0.02mg/kg,定量限(LOQ)为0.04mg/kg。鸡空白可食性组织中磺胺氯吡嗪添加样品在0.04～10.00 mg/kg范围内,平均回收率在75.46%～89.40%之间,批内和批间变异系数均小于9%。本试验建立的磺胺氯吡嗪提取和测定方法适用于鸡可食性组织中磺胺氯吡嗪残留量的定量分析。2.鸡可食性组织中甲氧苄啶残留量的高效液相色谱检测方法鸡可食性组织中甲氧苄啶残留采用乙腈提取、正己烷除脂、MCX固相萃取小柱净化,高效液相色谱紫外检测器检测。流动相为乙腈-0.01 mol/L磷酸二氢钾水溶液(18/82,v/v),紫外检测波长为240 nm。外标法定量。结果显示,甲氧苄啶在鸡可食性组织中检测限和定量限分别为0.01 mg/kg和0.025 mg/kg。甲氧苄啶标准溶液在0.05～8.00 μg/mL(0.025～4.00 mg/kg)浓度范围内,呈良好的线性关系(r0.9999)。鸡空白可食性组织中甲氧苄啶添加样品在0.025～4.000 mg/kg范围内,平均回收率在77.16%～90.88%之间,批内和批间变异系数均小于7%。本试验建立的甲氧苄啶提取和测定方法适用于鸡可食性组织中甲氧苄啶残留量的定量分析。3.磺胺氯吡嗪钠-甲氧苄啶可溶性粉在鸡体内残留消除研究磺胺氯吡嗪钠-甲氧苄啶可溶性粉按300 mg/L(以磺胺氯吡嗪钠计)的最大推荐剂量给健康商品黄羽肉鸡(公母各半)混饮,连续6d,分别于停药后4h(即零休药期)、1d、3d、7 d、12 d各随机抽取6只鸡屠宰,并采集肌肉、肝脏、肾脏及皮脂等可食性组织供药物残留检测用。分别采用经验证的鸡可食性组织中磺胺氯吡嗪和甲氧苄啶残留量的高效液相色谱法,检测停药后鸡可食性组织中磺胺氯吡嗪和甲氧苄啶的残留量。结果显示,停药后4 h磺胺氯吡嗪在肾脏中残留量最高,其次为皮脂、肝脏,肌肉最低;磺胺氯吡嗪在肌肉、肝脏、肾脏、皮脂中的残留量分别于停药后3d、3d、7 d、12 d时均低于国家规定的MRL(0.1 mg/kg)。停药后4 h甲氧苄啶在肾脏中残留量最高,其次为肝脏,皮脂和肌肉较低;甲氧苄啶在肌肉、肝脏、肾脏、皮脂中的残留量分别于停药后1d、1d、7 d、3d均低于国家规定的MRL(0.05 mg/kg)。研究表明,磺胺氯吡嗪和甲氧苄啶在肌肉和肝脏中消除均最快,磺胺氯吡嗪在肾脏和皮脂中消除最慢,甲氧苄啶在肾脏中消除最慢,肾脏和皮脂是磺胺氯吡嗪的残留把组织,肾脏是甲氧苄啶的残留靶组织。采用WT1.4软件拟合磺胺氯吡嗪和甲氧苄啶在肾脏和皮脂的休药期,得出停药后磺胺氯吡嗪在鸡肾脏、皮脂的休药期分别为15.47 d、18.18 d,甲氧苄啶在鸡肾脏和皮脂的休药期分别为9.08 d和13.69 d。综合残留消除试验结果,磺胺氯吡嗪钠-甲氧苄啶可溶性粉按推荐剂量饮水给药,休药期可暂定为19 d。
[Abstract]:Sulfachlorpyridazine sodium and trimethoprim soluble powder is a new compound, mainly used for veterinary clinical prevention and control of chicken coccidiosis. The edible chicken tissues (muscle, liver, kidney, sebum) in the residual marker sulfaclozine (SPZ) and trimethoprim (TMP) method for the detection of HPLC residues, elimination of residues in chicken tissues of sulfaclozine sodium soluble powder for trimethoprim, high performance liquid formulations of the new compound and provide a theoretical basis for the.1. chicken in the chicken Hugh medicine period residues sulfaclozine edible tissues by color spectrum detection method of chicken by using ammonia acetonitrile of sulfachlorpyridazine in the residual edible tissue samples (5/95, v/v) extract, hexane degreasing, MCX SPE column, high performance liquid chromatography with UV detector. The mobile phase was -0.02 mol/L KH2PO4 solution (35/ 65, v/v). The UV detection wave The length of 272 nm. and an external standard method. The results showed that sulfaclozine standard solution in 0.08 ~ 20 g/mL (0.04 ~ 10.00mg/kg) concentration range showed a good linear relationship (r0.9999). The detection limit (LOD) for 0.02mg/kg, the limit of quantification (LOQ) for 0.04mg/kg. chickens can add sulfachlorpyridazine of blank in edible tissues samples from 0.04 to 10 in the range of mg/kg, the average recovery rate was 75.46% ~ 89.40%, the coefficient of variation within and between the group were less than 9%. the sulfaclozine extraction and determination method for chicken chicken detection method of chromatography can be extracted by acetonitrile and trimethoprim residues in edible tissues by high performance liquid the quantitative analysis of.2. chicken residues in edible tissues of trimethoprim sulfaclozine residues in edible tissues, hexane degreasing, MCX SPE column, high performance liquid chromatography with UV detector. The mobile phase was -0.01 mol/ L KH2PO4 solution (18/82, v/v). The UV detection wavelength was 240 nm. using external standard method. The results showed that TMP in edible tissues of LOD and LOQ were 0.01 mg/kg and 0.025 mg/kg. standard solution in 0.05 ~ 8 and g/mL in chicken (0.025 ~ 4 mg/kg) concentration range, a a good linear relationship (r0.9999). The blank chicken can add trimethoprim edible tissues samples at 0.025 ~ 4 mg/kg range, the average recovery rate was 77.16% ~ 90.88%, the intra and inter coefficient of variation is less than 7%. the trimethoprim extraction and determination method for trimethoprim in edible chicken tissues the residual amount of quantitative analysis of.3. sulfaclozine sodium and trimethoprim soluble powder in chicken residue elimination of sulfachlorpyridazine sodium and trimethoprim soluble powder at 300 mg/L (with sulfaclozine sodium) the biggest push 鑽愬墏閲忕粰鍋ュ悍鍟嗗搧榛勭窘鑲夐浮(鍏�姣嶅悇鍗�)娣烽ギ,杩炵画6d,鍒嗗埆浜庡仠鑽�鍚�4h(鍗抽浂浼戣嵂鏈，

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