【摘要】：色譜法是現(xiàn)代分離分析的重要方法,作為其兩個(gè)重要分支,高效毛細(xì)管電泳(HPCE)法與高效液相色譜(HPLC)法以其準(zhǔn)確、高效的特點(diǎn),在人們?nèi)粘Ｉ钏褂玫氖称�、藥物的質(zhì)量和安全監(jiān)測(cè)等方面都有廣泛的應(yīng)用。本論文主要對(duì)HPCE法與HPLC法在食品、藥品中重屬離子檢測(cè)方面進(jìn)行了研究。本論文共分五章。第一章、總體介紹了高效毛細(xì)管電泳法和高效液相色譜法在食品及藥品中重屬離子檢測(cè)方面的應(yīng)用,以及論文的選題依據(jù)和主要研究?jī)?nèi)容。第二章、研究了毛細(xì)管電泳-間接紫外法,同時(shí)測(cè)定雙黃連口服液中Cd2+,Cr3+,Cu2+和Zn2+含量的方法。最佳分離體系:緩沖溶液為15 mmol/L咪唑(10 mol/L醋酸調(diào)節(jié)pH=4.5)。最佳分離條件為:0.5 psi壓力進(jìn)樣5 s,電壓20 kv,檢測(cè)波長(zhǎng)218 nm。該方法總檢測(cè)時(shí)間不超過6 min。四種重金屬離子線性范圍為0.5~35μg/mL,線性相關(guān)系數(shù)為0.9984~0.99999,檢出限0.08μg/mL~0.61μg/mL,加標(biāo)回收率94.2~103.8%。從對(duì)三種實(shí)際樣品的分析結(jié)果表明,方法操作簡(jiǎn)單,檢出限低,檢測(cè)速度快,適用于雙黃連口服液中重金屬離子的檢測(cè)分析。第三章、建立了柱前衍生HPLC法測(cè)定香煙中Ni2+和Cu2+含量的方法。使用二乙基二硫代氨基甲酸鈉(NaDDTC)作為柱前衍生劑,采用C-18反相色譜柱為固定相,甲醇:水(體積比75:25)為流動(dòng)相進(jìn)行檢測(cè)。結(jié)果如下:Ni2+和Cu2+的線性范圍為0.1~30μg/mL,線性相關(guān)系數(shù)為0.9988和0.9997,檢出限0.017和0.011μg/mL,加標(biāo)回收率96.83~104.50%。方法操作簡(jiǎn)單,檢出限低,適用于香煙中重金屬離子的檢測(cè)分析。第四章、建立了濕法消解處理樣品,在線衍生-反相HPLC法同時(shí)測(cè)定醬油中Pb2+和Ni2+含量的方法。二乙基二硫代氨基甲酸鈉(NaDDTC)為在線衍生試劑,C-18反相色譜柱為固定相,甲醇:水:衍生劑(體積比63.5:35:1.5)為流動(dòng)相,對(duì)重金屬進(jìn)行檢測(cè)。實(shí)驗(yàn)結(jié)果如下:Pb2+與Ni2+的線性范圍為0.5~50μg/mL,線性相關(guān)系數(shù)為0.9982和0.9990,檢出限為0.3μg/mL和0.2μg/mL,樣品加標(biāo)回收率88.1%~91.8%。方法操作簡(jiǎn)單,檢出限低,檢測(cè)速度快,適用于醬油中重金屬離子的檢測(cè)分析。第五章,研究了利用雙水楊醛鄰苯二胺希夫堿(SALOPHEN)作為衍生劑,結(jié)合HPLC法測(cè)定茶葉中Pb2+含量的方法。C-18反相色譜柱為固定相,甲醇:水(體積比80:20)為流動(dòng)相,檢測(cè)波長(zhǎng)226 nm。結(jié)果如下:Pb2+線性范圍為0.1~30μg/mL,線性相關(guān)系數(shù)為0.9988,檢出限為0.01μg/mL,加標(biāo)回收率為91.87~96.96%。方法操作簡(jiǎn)單,分析速度快,同時(shí)有較低的檢出限,適用于茶葉中Pb2+的檢測(cè)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.
【學(xué)位授予單位】：煙臺(tái)大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：O657.7;TS207.51;TQ460.72

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