色谱法用于食品及药品中重金属离子检测方法的研究

发布时间：2018-07-18 11:32

【摘要】：色谱法是现代分离分析的重要方法,作为其两个重要分支,高效毛细管电泳(HPCE)法与高效液相色谱(HPLC)法以其准确、高效的特点,在人们日常生活所使用的食品、药物的质量和安全监测等方面都有广泛的应用。本论文主要对HPCE法与HPLC法在食品、药品中重属离子检测方面进行了研究。本论文共分五章。第一章、总体介绍了高效毛细管电泳法和高效液相色谱法在食品及药品中重属离子检测方面的应用,以及论文的选题依据和主要研究内容。第二章、研究了毛细管电泳-间接紫外法,同时测定双黄连口服液中Cd2+,Cr3+,Cu2+和Zn2+含量的方法。最佳分离体系:缓冲溶液为15 mmol/L咪唑(10 mol/L醋酸调节pH=4.5)。最佳分离条件为:0.5 psi压力进样5 s,电压20 kv,检测波长218 nm。该方法总检测时间不超过6 min。四种重金属离子线性范围为0.5~35μg/mL,线性相关系数为0.9984~0.99999,检出限0.08μg/mL~0.61μg/mL,加标回收率94.2~103.8%。从对三种实际样品的分析结果表明,方法操作简单,检出限低,检测速度快,适用于双黄连口服液中重金属离子的检测分析。第三章、建立了柱前衍生HPLC法测定香烟中Ni2+和Cu2+含量的方法。使用二乙基二硫代氨基甲酸钠(NaDDTC)作为柱前衍生剂,采用C-18反相色谱柱为固定相,甲醇:水(体积比75:25)为流动相进行检测。结果如下:Ni2+和Cu2+的线性范围为0.1~30μg/mL,线性相关系数为0.9988和0.9997,检出限0.017和0.011μg/mL,加标回收率96.83~104.50%。方法操作简单,检出限低,适用于香烟中重金属离子的检测分析。第四章、建立了湿法消解处理样品,在线衍生-反相HPLC法同时测定酱油中Pb2+和Ni2+含量的方法。二乙基二硫代氨基甲酸钠(NaDDTC)为在线衍生试剂,C-18反相色谱柱为固定相,甲醇:水:衍生剂(体积比63.5:35:1.5)为流动相,对重金属进行检测。实验结果如下:Pb2+与Ni2+的线性范围为0.5~50μg/mL,线性相关系数为0.9982和0.9990,检出限为0.3μg/mL和0.2μg/mL,样品加标回收率88.1%~91.8%。方法操作简单,检出限低,检测速度快,适用于酱油中重金属离子的检测分析。第五章,研究了利用双水杨醛邻苯二胺希夫碱(SALOPHEN)作为衍生剂,结合HPLC法测定茶叶中Pb2+含量的方法。C-18反相色谱柱为固定相,甲醇:水(体积比80:20)为流动相,检测波长226 nm。结果如下:Pb2+线性范围为0.1~30μg/mL,线性相关系数为0.9988,检出限为0.01μg/mL,加标回收率为91.87~96.96%。方法操作简单,分析速度快,同时有较低的检出限,适用于茶叶中Pb2+的检测分析。
[Abstract]:Chromatography is an important method for modern separation and analysis. As two important branches of chromatography, high performance capillary electrophoresis (HPCE) and high performance liquid chromatography (HPLC) are used in people's daily life because of their accuracy and high efficiency. Drug quality and safety monitoring are widely used. In this paper, HPCE and HPLC were used to detect heavy ions in food and drug. This thesis is divided into five chapters. In the first chapter, the application of high performance capillary electrophoresis (HPCE) and high performance liquid chromatography (HPLC) in the detection of heavy ions in food and medicine is introduced, as well as the basis and main research contents of the thesis. In the second chapter, capillary electrophoresis and indirect ultraviolet spectrophotometry were used to determine the content of CD 2, Cr 3, Cu 2 and Zn 2 in Shuanghuanglian oral liquid. The optimum separation system was as follows: the buffer solution was 15 mmol / L imidazole (10 mol / L acetic acid adjusted pH = 4.5). The optimum separation conditions were as follows: 1: 0.5 psi pressure injection 5 s, voltage 20 kv, detection wavelength 218 nm. The total detection time of this method is not more than 6 mins. The linear range of the four heavy metal ions is 0.5 ~ 35 渭 g 路mL ~ (-1), the linear correlation coefficient is 0.9984 ~ 0.9999, the detection limit is 0.08 渭 g / mL ~ (-1) 0.61 渭 g 路mL ~ (-1), and the recovery rate is 94.2 渭 g 路mL ~ (-1). The results showed that the method was simple in operation, low in detection limit and rapid in detection. It was suitable for the determination of heavy metal ions in Shuanghuanglian oral liquid. In chapter 3, a HPLC method for the determination of Ni 2 and Cu 2 in cigarettes by pre-column derivatization was established. Sodium diethyldithiocarbamate (NaDDTC) was used as precolumn derivative, C-18 reversed phase column was used as stationary phase, and methanol: water (75:25 by volume) was used as mobile phase. The results showed that the linear range of 1: Ni2 and Cu2 was 0.1 渭 g / mL, the linear correlation coefficients were 0.9988 and 0.9997, the detection limits were 0.017 and 0.011 渭 g / mL, and the recoveries were 96.83 渭 g / mL and 104.50 respectively. The method is simple in operation and low in detection limit. It is suitable for the detection and analysis of heavy metal ions in cigarettes. In chapter 4, a method for simultaneous determination of Pb _ 2 and Ni _ 2 in soy sauce by on-line derivatization and reversed phase HPLC was established. Sodium diethyldithiocarbamate (NaDDTC) was used as an on-line derivative reagent and C-18 column as stationary phase, and methanol: water: derivative (63.5: 35: 1.5 by volume) as mobile phase to detect heavy metals. The results are as follows: the linear range of 0. 5 渭 g / mL for Pb 2 and Ni 2 is 0.5 渭 g / mL, the linear correlation coefficient is 0.9982 and 0. 9990, the detection limit is 0. 3 渭 g / mL and 0. 2 渭 g / mL, and the recovery rate is 88. 1 渭 g / mL and 91. 8 渭 g / mL respectively. The method is simple in operation, low in detection limit and fast in detection speed. It is suitable for the detection and analysis of heavy metal ions in soy sauce. In chapter 5, using bis-salicylaldehyde o-phenylenediamine Schiff base (SALOPHEN) as a derivative, the HPLC method for the determination of Pb _ 2 in tea was studied. The HPLC method was used as the stationary phase, methanol: water (80:20 by volume) as the mobile phase, and the detection wavelength was 226 nm. The results showed that the linear range of: PB2 was 0.1 渭 g / mL, the linear correlation coefficient was 0.9988, the detection limit was 0.01 渭 g / mL, and the recovery rate was 91.870.96%. The method is simple in operation, fast in analysis and low in detection limit. It is suitable for the detection and analysis of Pb 2 in tea.
【学位授予单位】：烟台大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O657.7;TS207.51;TQ460.72

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