苹果中三类植物生长调节剂残留的色谱分离分析方法研究

Study on the Chromatography Method for the Residue Determination of Three Types of Plant Growth Regulators in Apple

作者: 专业:分析化学 导师:张书胜 年度:2010 学位:硕士  院校: 郑州大学

Keywords

Plant growth regulators, High performance liquid chromatography, Ultra performance liquid chromatography - tandem mass spectrometry

        植物生长调节剂在现代农业、林业、果树、蔬菜及花卉生产中应用十分广泛,给人们的生产生活带来了巨大的利益。随着人们环保意识的增加,人们不仅注重作物的产量和营养,更加关注对环境的影响以及食品安全问题,对植物生长调节剂进行分析检测具有重大的实际意义。本课题主要采用高效液相色谱技术(HPLC)以及超高效液相色谱-质谱联用技术(UPLC-MS/MS),研究并建立了三类植物生长调节剂的分离分析方法,并对实际样品浓缩苹果汁中的三类植物生长调节剂含量进行了分析测定。本文主要进行了以下三方面的研究:1.建立了调吡脲、氯虫苯甲酰胺和除虫脲的HPLC-UV分离分析方法,通过对色谱分离柱、流动相组成、检测波长等色谱条件的优化,在8 min之内实现了三种物质的分离分析,检测限分别为0.02μg/mL、0.05μg/mL、0.13μg/mL,回收率在92.4%-103.9%之间。对浓缩苹果汁中的三种植物生长调节剂进行了定量分析,三种物质的含量为0.15-5.32μg/kg。2.通过对色谱分离柱、流动相组成、检测波长等色谱条件的优化,建立了吲哚丁酸、对氟苯氧乙酸、α-萘乙酸和2,4-D的HPLC-UV分离分析方法,这四种物质的保留时间分别为7.3 min,8.3 min、9.2 min、12.0 min,检测限分别为0.01μg/mL、0.05μg/mL、0.01μg/mL、0.05μg/mL;回收率在93.6%-115.3%之间。对实际样品进行分析,样品中四种物质的含量为0.21-5.52μg/kg。3.优化了缩节胺、矮壮素、青鲜素和多效唑的UPLC-MS/MS条件,通过对色谱分离柱、流动相组成、检测波长、洗脱方式、离子模式等色谱和质谱条件的优化,在1.5 min内实现了对四种物质的快速分析,并对四种物质的质谱裂解规律进行了解析。这四种物质的检测限分别为0.6μg/kg、0.7μg/kg、0.8μg/kg、0.8μg/kg;回收率在79.2%-103.6%之间。对实际样品进行分析,样品中四种物质的含量为0.83-4.29μg/kg。
    Plant growth regulators have wide range of applications in modern agriculture, forestry, fruit trees, vegetables and flower productions. They bring enormous benefits to people’s production and life. As the increase awareness of environmental protection, people not only focus on crop yields and nutrition, but also concern about the environment and food safety issues. Therefore, the analyses of plant growth regulators have important significance.With high performance liquid chromatography (HPLC) and ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), the three types of plant growth regulators analytical methods have been researched and established in this paper, which contain the following three aspects:We established a practical method for the separation and determination of forchlorfenuron, chlorantraniliprole and diflubenzuron by HPLC-UV. By the optimization of chromatographic separation column, mobile phase and the wavelength, three substances achieved baseline separation within 8 minutes. The detection limits were 0.02μg/mL,0.05μg/mL and 0.13μg/mL with recoveries between 92.4 and 103.9 percent. Three plant growth regulators in the concentrated apple juice for quantitative analysis were about 0.15-5.32μg/kg.With the optimization of chromatographic separation column, mobile phase and the wavelength, the HPLC-UV analytical method for four regulators,3-indole butyric acid,4-fluorophenoxyacetic acid, a-naphthaleneacetic acid and 2,4-D has been developed. The retention time of these four regulators were 7.3 min,8.3 min,9.2 min, and 12.0 min, respectively. The detection limits were 0.01μg/mL,0.05μg/mL,0.01μg/mL and 0.05μg/mL with the recovery between 93.6 and 115.3 percent. Four regulators in actual samples were 0.21-5.52μg/kg.The UPLC-MS/MS conditions have been optimized to analyze mepiquat chloride, chlormequat, paclobutrazol and maleic hydrazide by different chromatographic separation columns, mobile phases, detection wavelength, elution mode, ion mode chromatography and mass spectrometry conditions. Within 1.5 minutes four regulators were rapidly baseline separated and their mass spectroscopy character and fragmentation rules ware recommended. The detection limits of the four regulators were 0.6μg/kg,0.7μg/kg,0.8μg/kg and 0.8μg/kg with recoveries between 79.2 and 103.6 percent. Four regulators in actual samples were about 0.83-4.29μg/kg.
        

苹果中三类植物生长调节剂残留的色谱分离分析方法研究

摘要4-5
Abstract5
第一章 绪论10-18
    1 植物生长调节剂简介10
    2 植物生长调节剂的分类10-12
    3 蔬菜水果中常用植物生长调节剂的毒性、残留限量标准及残留现状12-14
    4 小结14-15
    参考文献15-18
第二章 苹果汁中调吡脲、氯虫苯甲酰胺和除虫脲残留的HPLC分析方法研究18-28
    1 前言18-20
        1.1 调吡脲、氯虫苯甲酰胺和除虫脲的理化性质和药效18-19
        1.2 调吡脲、氯虫苯甲酰胺和除虫脲研究进展19-20
    2 实验部分20-21
        2.1 试剂与溶液的配制20
        2.2 仪器和HPLC/UV条件20
        2.3 样品前处理20-21
            2.3.1 提取20
            2.3.2 净化20-21
    3 结果与讨论21-26
        3.1 前处理方法的考察21
        3.2 样品基质及标样的色谱图21-24
        3.3 回归方程、相关系数及检出限24
        3.4 回收率24-25
        3.5 重现性考察25-26
        3.6 实际样品的测定26
    4 小结26-27
    参考文献27-28
第三章 苹果汁中吲哚丁酸、对氟苯氧乙酸、α-萘乙酸、2,4-D残留的HPLC分析方法研究28-39
    1 前言28-30
        1.1 吲哚丁酸、对氟苯氧乙酸、α-萘乙酸和2,4-D的理化性质和药效28-29
        1.2 吲哚丁酸、对氟苯氧乙酸、α-萘乙酸和2,4-D的研究进展29-30
    2 实验部分30-31
        2.1 试剂与溶液的配制30
        2.2 仪器和HPLC/UV条件30-31
        2.3 样品前处理31
            2.3.1 提取31
            2.3.2 净化31
    3 结果与讨论31-36
        3.1 样品基质及标样的色谱图31-33
        3.2 回归方程、相关系数及检出限33-34
        3.3 回收率34-35
        3.4 重现性考察35-36
        3.5 实际样品的测定36
    4 小结36-37
    参考文献37-39
第四章 苹果汁中缩节胺、矮壮素、多效唑和青鲜素残留的UPLC-MS/MS分析方法研究39-57
    1 前言39-43
        1.1 缩节胺、矮壮素、多效唑和青鲜素的理化性质39-41
        1.2 由HPLC到UPLC的发展历程41-43
        1.3 缩节胺、矮壮素、多效唑和青鲜素的研究进展43
    2 实验部分43-45
        2.1 仪器和试剂43-44
        2.2 优化的UPLC/MS/MS条件44-45
        2.3 样品的提取净化处理45
            2.3.1 提取45
            2.3.2 净化45
        2.4 标准溶液的配制45
    3 结果与讨论45-56
        3.1 确定分析条件45-46
            3.1.1 质谱最佳分离条件的确定45
            3.1.2 色谱最佳分离条件的确定45-46
        3.2 缩节胺、矮壮素、青鲜素和多效唑的ESI/MS和ESI/MS/MS分析46-51
        3.3 标准品的UPLC-ESI/MS/MS分析51-55
        3.4 标准曲线和检出限55
        3.5 回收率和精密度55-56
        3.6 样品测定结果56
    4 小结56-57
全文结论57-58
参考文献58-60
硕士期间发表的文章60-61
致谢61
        下载全文需10


本文地址:

上一篇:纳米金修饰电极的制备与应用研究
下一篇:锰氧化物改性沸石(MOCZ)对罗丹明B和4-氯苯酚的吸附研究

分享到: 分享苹果中三类植物生长调节剂残留的色谱分离分析方法研究到腾讯微博           收藏
评论排行
公告