| Arsenic is a toxic substance which has been reported with the the incidence of many types of cancer and disease. Inorganic Arsenic has been classified as strong carcinogenic substances by International Cancer Research Commission. Arsenic toxicity is not only related with the total arsenic content,but the elements of the chemical form of closely related. At present, we still stuck in the detection of total arsenic, and can not correctly evaluate the arsenic hazards to human. Form of separation of arsenic in food analysis techniques for the monitoring of arsenic contamination and residual issues has become imperative.This project used high performance liquid chromatography-inductively coupled plasma mass spectrometry analysis of food of animal origin roxarsone, arsanilic acid and nitric acid phenyl arsine, and improved pre-treatment methods. This method used methanol as aqueous solution on the sample pre-treatment. Respectively, using methanol-water solution and artificial gastric juice enzyme pre-treatment samples and founded that the proportion of aqueous methanol to extract the best is1:9, artificial gastric juice enzymatic method could achieve the same effect. Since methanol is toxic, We ended up with artificial gastric juice enzymatic hydrolysis.This project used high-performance liquid chromatography-inductively coupled plasma mass spectrometry detection method for the simultaneous analysis of seven kinds of arsenic species in food of animal origin. The introduction of artificial gastric juice enzymatic pretreatment methods solved the problem of methanol water extraction of high-protein sample matrix arsenite recovery rate is low,and using gradient elution to achieve a good separation of seven arsenic species.Added by feeding experiments on animal (Sanhuang) muscle, liver, skin and blood in roxarsone, arsanilic acid and its metabolites were measured.and determines the residue characterization of Arsenic and its metabolites in tissues of animals and residual marker, the simultaneous determination of animal liver pathology test and blood biochemical indicators. The results showed that①Types of metabolites: Arsanilic acid to add the group in various tissues residues of arsenic species were arsanilic acid, dimethyl arsenic and arsenite; The Roxarsone adding a group mainly included roxarsone, a methyl arsenic and dimethyl arsenic, arsenite and arsenate. Types of metabolites were more than arsanilic acid’s, and the proportion of arsenic species in different parts of the organization had a great deal of difference.②etabolic rate:The metabolism in the liver and blood is faster, while the slowest in the skin.The same concentration level of arsanilic acid metabolism was fast and relatively thorough,while roxarsone metabolism was complex and slow, and overall drug residues was higher than arsanilic acid.③Residue characterization: Organization site residue characterization adding the arsanilic acid group were arsanilic acid, dimethyl arsenic and arsenite; The site residue characterization adding roxarsone in the muscles were roxarsone, dimethyl arsenic and arsenite, in the livers were roxarsone, dimethyl arsenic, arsenite and methyl arsenic, and in the blood were roxarsone, dimethyl arsenic, arsenite and arsenate.④Residual markers:dimethyl arsenic and arsenite.⑤Lver pathology test:the higher adding concentration the more obvious symptoms of liver diseases, and the colors gradually deepened.The higher concentration adding group visible swellings Seriously and bleedings obviously,and had the trends of cirrhosis and liver tumors.⑥Setermination of blood biochemical parameters:It could improve the activity of alanine aminotransferase, aspartate aminotransferase, and alkaline phosphatase in chicken plasma. The higher the adding concentration, the more obviously the effect,and the influence to Alanine aminotransferase was the most significant.This project tested arsenic in the fruits and vegetables, aquatic products and other food by seven arsenic species detection methods which have studied, and established a high efficiency liquid chromatography-inductively coupled plasma mass spectrometry determination of food (meat, fruits and vegetables and aquatic products) and the detection of six arsenic species.The project improved the detection of food of animal origin, roxarsone, arsanilic acid and nifedipine Arsenoxylphenylazo methods (HPLC-ICP-MS) in the pre-treatment technology by using morphological analysis as the main means of research.We established detection method (HPLC-ICP-MS)on the simultaneous analysis of arsenic species in food of animal origin and extended the application of six kinds of arsenic species in food detection (HPLC-ICP-MS). The systematic studies of arsenic and its metabolites in animals determine the residual characterization and residual marker of Arsenic and its metabolites in various organizations of the animals. This project filled the blank of the international and domestic research in this field and provided technical supports for law enforcement to ensure smoothly export-inspection and quarantine of food of animal origin. |
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