| 3-monochloro-1,2-propanediol(3-MCPD)has reproductive toxicity,renal toxicity,neurotoxicity,genotoxicity,carcinogenicity and other toxicity,which is classified as class 2B carcinogen by the international agency for research on cancer(IARC).Currently,the detection methods of 3-MCPD mainly include gas chromatography(GC),gas chromatography-mass spectrometry(GC-MS),capillary electrophoresis(CE),molecular imprinting(MIP),etc.This topic is based on the laboratory has established the adenine derivative,on the basis of 3-MCPD,three kinds of derivatives of adenine ninth replace with 3-MCPD after derivatization of derivative fluorescence spectrum analyses,finally determine the hydroxypropyl adenine derivative work better as derivative reagent,and free in the environment of water and edible vegetable oil 3-MCPD are well on the test application.This topic mainly includes the following parts:(1)Chloroacetaldehyde iminodiacetic acid hydrolysis aldehyde chloroacetaldehy-de were obtained with adenine,methyl adenine,hydroxyethyl adenine,hydroxypropyl adenine reaction,using HPLC-UV separation.Four 3-MCPD derivatives,through exploring its fluorescence intensity and p H,methanol volume fraction,the relationship between the concentration of NaCl,determine the method of HPLC-FLD—the best separation conditions,finally it is concluded that hydroxypropyl adenine derivative effect is better.(2)The generation of the blank peak inhibition of exploring experiments show that based on sodium periodate oxidation cracking 3-MCPD,excess sodium sulfite and sodium periodate added on the basis of the formation of lead acetate can effectively restrain blank peak,derivative reagent p H and concentration,the oxidative cracking time,derivative temperature and time of the single factor experiments to further improve the sensitivity of the method.(3)In the pure water system,the standard curve equations of 0.0～100.0ng/mL and 100.0～1000.0ng/mL 3-MCPD are y=7.91447x+27.43477 and y=7.62336x+40.83123,respectively.R~2 was 0.9974 and 0.9974,respectively.Lake water,river water and paper mill water were taken as the test samples of 3-MCPD in environmental water,and the contents of 3-MCPD were 0.52μg/kg、1.47μg/kg and3.51μg/kg,respectively.(4)In the 0.03g/mL NaCl solution system,the standard curve equation of 0～100ng/mL 3-MCPD is y=7.83635x+24.82129,R~2=0.99863.The extraction method of free3-MCPD in edible vegetable oil established in the laboratory was modified,and the3-MCPD content in soybean oil,rice oil,peanut oil,camellia oil and corn oil were determined as 16.37μg/kg、26.89μg/kg、153.74μg/kg、30.51μg/kg and 17.48μg/kg respectively.(5)Based on the laboratory adenine-derived 3-MCPD method applied to the detection of 3-MCPD in soy sauce,it was found that sucralose would have a great impact on the experimental results.The exploratory experiment of separating3-MCPD and sucralose in soy sauce by dialysis bag showed that the pretreatment effect was poor. |
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