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HPLC-CL Method For The Determination Of Trace Amount Of Food Additives

Posted on:2012-11-02Degree:MasterType:Thesis
Country:ChinaCandidate:Y Q YuanFull Text:PDF
GTID:2131330332486218Subject:Applied Chemistry
Abstract/Summary:PDF Full Text Request
This topic combined highly sensitive chemiluminescent detection technology with high-performance high performance liquid chromatography technology in an appropriate manner, and established common detection methods of common food additives.This paper mainly discussed chemiluminescence reaction and chromatographic analysis conditions. By one-factor analysis, the effect of amount of chemiluminescence reagents and chemical oxidants and so on were investigated, moreover the effect of mobile phase, flow rate, column temperature, the detection wavelength and sampling volume were also investigated in detail.Under the optimized chemiluminescence reaction and chromatography analysis conditions, HPLC-CL methods for the determination of vanillin, Sudan I, vitamin C, and benzoyl peroxide were established successfully.Linear range, precision, detection limit and accuracy were researched one by one. The new methods were used to the determination of the corresponding components in food to examine the feasibilities of the methods. In addition, the reproducibilities of the methods were also checked by testing the real samples.In alkaline condition, vanillin can enhance the CL intensity of LC-H2O2-NaOH system.Based on this,a new analytical method of HPLC-CL for vanillin was established and successfully applied to the determination of vanillin in food. The results showed that a good linear relationship exists between the CL intensity and the concentration of vanillin in the range of 1.0~20.0μg·mL-1, the regression equation was I=8.539+2.953×106C, the correlation coefficient was 0.9921, the precision was 1.97%(c= 8.0μg·mL-1, n=6), the detection limit was 3ng·mL-1 and the recovery was 98.2~103.3%, the present method was proved to be rapid, sensitive and feasible in real sample test.In alkaline condition, a new method of high performance liquid chromatography chemiluminescence determination of Sudan I was established,based on Sudan I to increase the intensity of luminol-KIO4 system. The results showed that a good linear relationship exists between the CL intensity and the concentration of Sudan I in the range of 0.001~0.50μg·mL-1,The regression equation was I=8.393×103C+224.5(R=0.9996).The detection limit was 5 ng·kg-1 and the relative standard deviation is 1.45%(c=0.01μg·mL-1, n=6). The recovery was in the range of 95.0%~104.0%,the new method was proved to be rapid, sensitive and feasible in real sample test.It has been found that chromium (Ⅲ) from the reduction of Vc and potassium dichromate can catalyze luminol chemiluminescence reaction. Based on this,a new method for Vc was established. The results showed that a good linear relationship exists between the CL intensity and the concentration of vitamin C in the range of 0.01~10.0μg·mL-1, the regression equation was I= 2.383×103C+393.6, the correlation coefficient (R) was 0.9979, the precision was 1.57%(c=6.0μg·mL-1, n=6), the detection limit was 0.5ng·mL-1 and the recovery was 94.6~102.0%, the new method of Vc was proved to be rapid, sensitive and feasible in real sample test.The study found that benzoyl peroxide could increase luminol-KMnO4 system intensity. According to this,the paper established a new method for benzoyl peroxide determination. The results show that a good linear relationship exists between the CL intensity and the concentration of benzoyl peroxide in the range of 1.0~100.0μg·mL-1 with the regression equation of I=1.0427 X 104C+51.28, the correlation coefficient (R) was 0.9971, the precision was 2.1%(c= 10.0μg·mL-1, n=6), the detection limit was 0.2mg·g-1 and the recovery was 97.5~99.2%.
Keywords/Search Tags:HPLC, CL HPCL-CL, Vanillin, SudanⅠ, vitamin C, benzoyl peroxide, food
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