本文選題：磺胺氯吡嗪鈉-甲氧芐啶可溶性粉　切入點(diǎn)：雞　出處：《揚(yáng)州大學(xué)》2017年碩士論文

【摘要】：磺胺氯吡嗪鈉-甲氧芐啶可溶性粉是一種復(fù)方新制劑,獸醫(yī)臨床上主要用于防控雞球蟲病。本實(shí)驗(yàn)通過建立雞可食性組織(肌肉、肝臟、腎臟、皮脂)中殘留標(biāo)示物磺胺氯吡嗪(SPZ)和甲氧芐啶(TMP)殘留量的HPLC檢測方法,研究磺胺氯吡嗪鈉-甲氧芐啶可溶性粉在雞組織中的殘留消除規(guī)律,為制訂該復(fù)方新制劑在雞的休藥期提供理論依據(jù)。1.雞可食性組織中磺胺氯吡嗪殘留量的高效液相色譜檢測方法雞可食性組織樣品中磺胺氯吡嗪殘留采用氨水-乙腈(5/95,v/v)提取,正己烷除脂,MCX固相萃取小柱凈化,高效液相色譜紫外檢測器檢測。流動相為乙腈-0.02 mol/L磷酸二氫鉀水溶液(35/65,v/v),紫外檢測波長為272 nm。外標(biāo)法定量。結(jié)果顯示,磺胺氯吡嗪標(biāo)準(zhǔn)溶液在0.08～20.00 μg/mL(0.04～10.00mg/kg)濃度范圍內(nèi),呈良好的線性關(guān)系(r0.9999)。檢測限(LOD)為0.02mg/kg,定量限(LOQ)為0.04mg/kg。雞空白可食性組織中磺胺氯吡嗪添加樣品在0.04～10.00 mg/kg范圍內(nèi),平均回收率在75.46%～89.40%之間,批內(nèi)和批間變異系數(shù)均小于9%。本試驗(yàn)建立的磺胺氯吡嗪提取和測定方法適用于雞可食性組織中磺胺氯吡嗪殘留量的定量分析。2.雞可食性組織中甲氧芐啶殘留量的高效液相色譜檢測方法雞可食性組織中甲氧芐啶殘留采用乙腈提取、正己烷除脂、MCX固相萃取小柱凈化,高效液相色譜紫外檢測器檢測。流動相為乙腈-0.01 mol/L磷酸二氫鉀水溶液(18/82,v/v),紫外檢測波長為240 nm。外標(biāo)法定量。結(jié)果顯示,甲氧芐啶在雞可食性組織中檢測限和定量限分別為0.01 mg/kg和0.025 mg/kg。甲氧芐啶標(biāo)準(zhǔn)溶液在0.05～8.00 μg/mL(0.025～4.00 mg/kg)濃度范圍內(nèi),呈良好的線性關(guān)系(r0.9999)。雞空白可食性組織中甲氧芐啶添加樣品在0.025～4.000 mg/kg范圍內(nèi),平均回收率在77.16%～90.88%之間,批內(nèi)和批間變異系數(shù)均小于7%。本試驗(yàn)建立的甲氧芐啶提取和測定方法適用于雞可食性組織中甲氧芐啶殘留量的定量分析。3.磺胺氯吡嗪鈉-甲氧芐啶可溶性粉在雞體內(nèi)殘留消除研究磺胺氯吡嗪鈉-甲氧芐啶可溶性粉按300 mg/L(以磺胺氯吡嗪鈉計)的最大推薦劑量給健康商品黃羽肉雞(公母各半)混飲,連續(xù)6d,分別于停藥后4h(即零休藥期)、1d、3d、7 d、12 d各隨機(jī)抽取6只雞屠宰,并采集肌肉、肝臟、腎臟及皮脂等可食性組織供藥物殘留檢測用。分別采用經(jīng)驗(yàn)證的雞可食性組織中磺胺氯吡嗪和甲氧芐啶殘留量的高效液相色譜法,檢測停藥后雞可食性組織中磺胺氯吡嗪和甲氧芐啶的殘留量。結(jié)果顯示,停藥后4 h磺胺氯吡嗪在腎臟中殘留量最高,其次為皮脂、肝臟,肌肉最低;磺胺氯吡嗪在肌肉、肝臟、腎臟、皮脂中的殘留量分別于停藥后3d、3d、7 d、12 d時均低于國家規(guī)定的MRL(0.1 mg/kg)。停藥后4 h甲氧芐啶在腎臟中殘留量最高,其次為肝臟,皮脂和肌肉較低;甲氧芐啶在肌肉、肝臟、腎臟、皮脂中的殘留量分別于停藥后1d、1d、7 d、3d均低于國家規(guī)定的MRL(0.05 mg/kg)。研究表明,磺胺氯吡嗪和甲氧芐啶在肌肉和肝臟中消除均最快,磺胺氯吡嗪在腎臟和皮脂中消除最慢,甲氧芐啶在腎臟中消除最慢,腎臟和皮脂是磺胺氯吡嗪的殘留把組織,腎臟是甲氧芐啶的殘留靶組織。采用WT1.4軟件擬合磺胺氯吡嗪和甲氧芐啶在腎臟和皮脂的休藥期,得出停藥后磺胺氯吡嗪在雞腎臟、皮脂的休藥期分別為15.47 d、18.18 d,甲氧芐啶在雞腎臟和皮脂的休藥期分別為9.08 d和13.69 d。綜合殘留消除試驗(yàn)結(jié)果,磺胺氯吡嗪鈉-甲氧芐啶可溶性粉按推薦劑量飲水給藥,休藥期可暫定為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瘝鍚勫崐)娣烽ギ,榪炵畫6d,鍒嗗埆浜庡仠鑽悗4h(鍗抽浂浼戣嵂鏈，

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