性激素类兽药的化学发光分析研究
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摘要
激素是一类对机体功能起调节作用的化学物质，在农牧业、医药业等行业有着广泛的应用。由于激素的副作用，很多激素在牲畜饲养中被禁止使用。化学发光分析法作为一种灵敏快速的检测方法近年来在激素的分析应用中日益受到人们的重视。
本论文分为两个部分：综述和研究报告。
在综述部分，综述了近年来化学发光法在类固醇激素类药物分析中的应用。
在研究报告部分，研究了四种性激素类药物甲睾酮、丙酸睾酮、苯丙酸诺龙和去甲雄三烯醇酮(群勃龙)在高锰酸钾体系中的化学发光行为，仔细优化了实验条件，建立了测定甲睾酮、丙酸睾酮、苯丙酸诺龙和去甲雄三烯醇酮的化学发光新方法。同时，简单讨论了化学发光反应的机理。具体内容如下：
一、流动注射化学发光法测定甲睾酮、丙酸睾酮和苯丙酸诺龙
研究发现，甲睾酮、丙酸睾酮以及苯丙酸诺龙和浓硫酸的反应产物可以与酸性高锰酸钾反应产生弱的化学发光，醋酸奎宁的存在能使体系的化学发光强度显著增强。据此，对实验条件进行了优化，建立了测定甲睾酮、丙酸睾酮和苯丙酸诺龙的化学发光新方法。该方法的线性范围分别为5．0×10~(-8)-1．0×10~(-5)g／mL甲睾酮，5．0×10~(-8)-1．0×10~5g／mL丙酸睾酮和2．0×10~(-7)-5．0×10~(-5)g／mL苯丙酸诺龙；检出限分别为3×10~(-8)g／mL甲睾酮，4×10~(-8)g／mL丙酸睾酮和1×10~(-7)g／mL苯丙酸诺龙。对浓度为5．0×10~(-7)g／mL甲睾酮溶液，5．0×10~(-7)g／mL丙酸睾酮溶液和5．0×10~(-6)g／mL苯丙酸诺龙溶液分别进行11次平行测定，相对标准偏差分别为3．0％，4．3％和4．0％。该方法已应用于鱼肉中甲睾酮的含量测定。
二、流动注射化学发光法测定去甲雄三烯醇酮
研究发现，去甲雄三烯醇酮可以与KMnO_4反应产生弱的化学发光，茜素黄R的存在能显著增强体系的化学发光强度。基于此发现，建立了测定去甲雄三烯醇酮的化学发光新方法。该方法测定去甲雄三烯醇酮的线性范围1．0×10~(-7)-1．0×10~(-4)g／mL：检出限为5×10~(-8)g／mL。对浓度为2．0×10~(-6)g／mL去甲雄三烯醇酮溶液进行11次平行测定，相对标准偏差1．5％。该法已应用于饲料中去甲雄三烯醇酮的含量测定。
三、流动注射化学发光法测定盐酸氟桂利嗪
研究发现，在酸性条件下，盐酸氟桂利嗪与高锰酸钾反应可产生弱的化学发光，甲醛的存在对这一反应的化学发光强度具有显著的增强作用。据此，优化了化学发光反应条件，建立了测定盐酸氟桂利嗪的流动注射化学发光分析法。盐酸氟桂利嗪浓度与化学发光强度在8．0×10~(-7)-8．0×10~(-5)g／mL范围内具有线性关系。该方法的检出限为8×10~(-7)g／mL盐酸氟桂利嗪。对1．0×10~(-5)g／mL盐酸氟桂利嗪标准溶液进行11次平行测定的相对标准偏差为2．2％。该方法已用于盐酸氟桂利嗪胶囊中盐酸氟桂利嗪的含量测定。
Hormones are chemicals, which can adjust the body's function. They are widely used in agriculture, pharmaceutical and other industries. However, many hormones in the feed additive has been banned, because of the side effects of hormones. Chemiluminescence(CL) analysis as a sensitive and rapid detection method has attracted prople's attention in hormones analysis in recent years.
The thesis consists of review and research section.
In the review section, the analytical application of CL method in hormone analysis were summarized. In research report section, the CL behaviors of four sexual hormone in potassium permanganate system was studied. The experimental conditions were carefully optimized and a new flow injection CL method for the determination of four sexual hormone, namely methyltestosterone, testosterone propionate, nandrolone phenylpropionate and trenbolone, was proposed. The reaction mechanism was also briefly discussed
The research report section includes three parts.
Part one, a flow injection chemiluminescence method was proposed for the determination of methyltestosterone, testosterone propionate and nandrolone phenylpropionate. It was found that chemiluminescence was produced during the oxidation of the reaction product of methyltestosterone, testosterone propionate and nandrolone phenylpropionate with sulfuric acid by potassium permanganate in acidic condition. In the presence of quinine acetate, the CL signal was enhanced significantly. Under the optimum experimental conditions The linear ranges of the method were5.0×10~(-8)-1.0×10~(-5)g/mL methyltestosterone, 5.0×10~(-8)-1.0×10~(-5)g/mL testosterone propionate and 2.0×10~(-7)-5.0×10~(-5)g/mL nandrolone phenylpropionate. The detection limits were 3×10~(-8)g/mL methyltestosterone, 4×10~(-8)g/mL testosterone propionate and 1×10~(-7)g/mL nandrolone phenylpropionate. The relative standard deviations(n=11) were 3.0%, 4.3% and 4.0% for 5.0×10~(-7)g/mL methyltestosterone solution, 5.0×10~(-7)g/mL testosterone propionate solution and 5.0×10~(-6)g/mL nandrolone phenylpropionate solution, respectively. This method has been applied to the determination of androgens in fish with satisfactory results.
Part two, a new CL method was proposed for the determination of trenbolone. It was based on the CL reaction of trenbolone with potassium permanganate in the hydrochloric acid solution. The CL signal was enhanced greatly by alizarin yellow R. The CL signal was proportional to the trenbolone concentration in the range of 1.0×10~(-7)-1.0×10~(-4)g/mL. The detection limit was 5×10~(-8)g/mL trenbolone. The relative standard deviation was 1.5% for 2.0×10~(-6)g/mL trenbolone solution in eleven repeated measurements. This method has been applied to the determination of trenbolone in cattle feeds with satisfactory results.
Part three, weak CL signal is observed during the reaction of potassium permanganate with flunarizine hydrochloride in acid solution. In the presence of formaldehyde, the CL signal was enhanced significantly. Based on these phenomena, the experimental conditions that affected the CL reaction were optimized and a new flow injection CL method for the determination of flunarizine hydrochloride was proposed. The CL signal was linearly dependent on the concentration of flunarizine hydrochloride in the range of 8.0×10~(-7)-8.0×10~(-5)g/mL. The detection limits was 8xxxxx10~(-7) g/mL flunarizine hydrochloride and the relative standard deviation was 2.2% for 1.0×10~(-5)g/mL flunarizine hydrochloride solution in eleven repeated measurements. The proposed method was successfully applied to the determination of flunarizine hydrochloride in capsules.
本论文分为两个部分：综述和研究报告。
在综述部分，综述了近年来化学发光法在类固醇激素类药物分析中的应用。
在研究报告部分，研究了四种性激素类药物甲睾酮、丙酸睾酮、苯丙酸诺龙和去甲雄三烯醇酮(群勃龙)在高锰酸钾体系中的化学发光行为，仔细优化了实验条件，建立了测定甲睾酮、丙酸睾酮、苯丙酸诺龙和去甲雄三烯醇酮的化学发光新方法。同时，简单讨论了化学发光反应的机理。具体内容如下：
一、流动注射化学发光法测定甲睾酮、丙酸睾酮和苯丙酸诺龙
研究发现，甲睾酮、丙酸睾酮以及苯丙酸诺龙和浓硫酸的反应产物可以与酸性高锰酸钾反应产生弱的化学发光，醋酸奎宁的存在能使体系的化学发光强度显著增强。据此，对实验条件进行了优化，建立了测定甲睾酮、丙酸睾酮和苯丙酸诺龙的化学发光新方法。该方法的线性范围分别为5．0×10~(-8)-1．0×10~(-5)g／mL甲睾酮，5．0×10~(-8)-1．0×10~5g／mL丙酸睾酮和2．0×10~(-7)-5．0×10~(-5)g／mL苯丙酸诺龙；检出限分别为3×10~(-8)g／mL甲睾酮，4×10~(-8)g／mL丙酸睾酮和1×10~(-7)g／mL苯丙酸诺龙。对浓度为5．0×10~(-7)g／mL甲睾酮溶液，5．0×10~(-7)g／mL丙酸睾酮溶液和5．0×10~(-6)g／mL苯丙酸诺龙溶液分别进行11次平行测定，相对标准偏差分别为3．0％，4．3％和4．0％。该方法已应用于鱼肉中甲睾酮的含量测定。
二、流动注射化学发光法测定去甲雄三烯醇酮
研究发现，去甲雄三烯醇酮可以与KMnO_4反应产生弱的化学发光，茜素黄R的存在能显著增强体系的化学发光强度。基于此发现，建立了测定去甲雄三烯醇酮的化学发光新方法。该方法测定去甲雄三烯醇酮的线性范围1．0×10~(-7)-1．0×10~(-4)g／mL：检出限为5×10~(-8)g／mL。对浓度为2．0×10~(-6)g／mL去甲雄三烯醇酮溶液进行11次平行测定，相对标准偏差1．5％。该法已应用于饲料中去甲雄三烯醇酮的含量测定。
三、流动注射化学发光法测定盐酸氟桂利嗪
研究发现，在酸性条件下，盐酸氟桂利嗪与高锰酸钾反应可产生弱的化学发光，甲醛的存在对这一反应的化学发光强度具有显著的增强作用。据此，优化了化学发光反应条件，建立了测定盐酸氟桂利嗪的流动注射化学发光分析法。盐酸氟桂利嗪浓度与化学发光强度在8．0×10~(-7)-8．0×10~(-5)g／mL范围内具有线性关系。该方法的检出限为8×10~(-7)g／mL盐酸氟桂利嗪。对1．0×10~(-5)g／mL盐酸氟桂利嗪标准溶液进行11次平行测定的相对标准偏差为2．2％。该方法已用于盐酸氟桂利嗪胶囊中盐酸氟桂利嗪的含量测定。
Hormones are chemicals, which can adjust the body's function. They are widely used in agriculture, pharmaceutical and other industries. However, many hormones in the feed additive has been banned, because of the side effects of hormones. Chemiluminescence(CL) analysis as a sensitive and rapid detection method has attracted prople's attention in hormones analysis in recent years.
The thesis consists of review and research section.
In the review section, the analytical application of CL method in hormone analysis were summarized. In research report section, the CL behaviors of four sexual hormone in potassium permanganate system was studied. The experimental conditions were carefully optimized and a new flow injection CL method for the determination of four sexual hormone, namely methyltestosterone, testosterone propionate, nandrolone phenylpropionate and trenbolone, was proposed. The reaction mechanism was also briefly discussed
The research report section includes three parts.
Part one, a flow injection chemiluminescence method was proposed for the determination of methyltestosterone, testosterone propionate and nandrolone phenylpropionate. It was found that chemiluminescence was produced during the oxidation of the reaction product of methyltestosterone, testosterone propionate and nandrolone phenylpropionate with sulfuric acid by potassium permanganate in acidic condition. In the presence of quinine acetate, the CL signal was enhanced significantly. Under the optimum experimental conditions The linear ranges of the method were5.0×10~(-8)-1.0×10~(-5)g/mL methyltestosterone, 5.0×10~(-8)-1.0×10~(-5)g/mL testosterone propionate and 2.0×10~(-7)-5.0×10~(-5)g/mL nandrolone phenylpropionate. The detection limits were 3×10~(-8)g/mL methyltestosterone, 4×10~(-8)g/mL testosterone propionate and 1×10~(-7)g/mL nandrolone phenylpropionate. The relative standard deviations(n=11) were 3.0%, 4.3% and 4.0% for 5.0×10~(-7)g/mL methyltestosterone solution, 5.0×10~(-7)g/mL testosterone propionate solution and 5.0×10~(-6)g/mL nandrolone phenylpropionate solution, respectively. This method has been applied to the determination of androgens in fish with satisfactory results.
Part two, a new CL method was proposed for the determination of trenbolone. It was based on the CL reaction of trenbolone with potassium permanganate in the hydrochloric acid solution. The CL signal was enhanced greatly by alizarin yellow R. The CL signal was proportional to the trenbolone concentration in the range of 1.0×10~(-7)-1.0×10~(-4)g/mL. The detection limit was 5×10~(-8)g/mL trenbolone. The relative standard deviation was 1.5% for 2.0×10~(-6)g/mL trenbolone solution in eleven repeated measurements. This method has been applied to the determination of trenbolone in cattle feeds with satisfactory results.
Part three, weak CL signal is observed during the reaction of potassium permanganate with flunarizine hydrochloride in acid solution. In the presence of formaldehyde, the CL signal was enhanced significantly. Based on these phenomena, the experimental conditions that affected the CL reaction were optimized and a new flow injection CL method for the determination of flunarizine hydrochloride was proposed. The CL signal was linearly dependent on the concentration of flunarizine hydrochloride in the range of 8.0×10~(-7)-8.0×10~(-5)g/mL. The detection limits was 8xxxxx10~(-7) g/mL flunarizine hydrochloride and the relative standard deviation was 2.2% for 1.0×10~(-5)g/mL flunarizine hydrochloride solution in eleven repeated measurements. The proposed method was successfully applied to the determination of flunarizine hydrochloride in capsules.
引文
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