| 3-MCPD is another worrisome contaminants in the food industry after dioxins. Itcan poison the nervous system and circulatory system, damage the wall of kidneytubule, cause diabetes, increase the mass of liver and then cause hepatitis. It is alsoteratogenic and carcinogenic.Especially destructing the animal’s reproductive system,reducing sperm’s activity and content. As another worrisome contaminants in the foodindustry, it has been taken attention by international food industry.At present, there are increasing number of research on3-MCPD internationally,particularly focusing on the determination method of3-MCPD. The main directionsare pointed to the selection of suitable extraction and purification methods for3-MCPD, and the determination of its derivatives by varying derivatized chemicalagents. The methods of determination range from the primary gas chromatography(GC) to the gas chromatography-mass spectrometry (GC-MS), or other molecularimaging technology, and so forth.Generally speaking, however, these methodologiesare tedious, highly expensive, lower sensitivity, and they are at the disadvantage to themid-size and small businesses for the determination and control of3-MCPD.The paper presents a method to set up the high performance liquidchromatography with fluorescence detection (HPLC-FLD) for the quantitativedetermination of3-MCPD in the water samples. The method is simple to operate, lowcost, high selectivity and sensitivity. The costs of the instruments and facility arerelatively lower. The themes of the paper consist of the following subjects:(1) Derivatization reagent of three filter(OPD、1-amino-isoquinoline、2-amino-quinoline), the results show that2-aminoquinoline with good selectivity,high sensitivity, and can be used as3-MCPD derivatized new derivatization reagents.(2) Pretreated fatty acid esters of3-chloropropane-1,2-diol (3-MCPD) will beoxidized to chloroacetaldehyde with sodium periodate. And chloroacetaldehyde willderivatized with2-aminoquinoline (2-AQ) in fluorescence, producing vinyl-2-aminoquinoline(εEAQ) which has strong fluorescence under certain conditions. Afterthat, using it as the target peak for the chromatographic quantitative analysis of3-MCPD.The analysis results show that when the mobile phase of HPLC isacetonitrile-tris/HCl buffer(pH10,30-77，v/v), the appearance time of2-AQ andεEAQ are12.5min and18.7min. As their appearance time is quite different, is easy to separate them.(3) In order to improve the detection sensitivity better, this experiment willoptimize the detection conditions and reaction conditions. According to the results offluorescence scanning, Excitation and emission wavelengths of2-AQ and εEAQ aredifferent, so set excitation wavelength at λEX=234and emission wavelength atλEM=234could improve the response value target of detection.(4) Draw standard curve of3-MCPD under the optimized conditions.Theregression equations between the two concentration range of50ng/mL and1000ng/mL are y=2.290x+11.885and y=2.374x+3.698, their linear regressioncoefficients are0.998and0.997, that’s to say they have a good linear relationship.Verification results show that the experimental reproducibility and precision is verygood, and it can be applied to the detection of3-MCPD in environmental water.3-MCPD in tap water、 river water and water near the paper mill are2.4μg/kg、6.6μg/kg and11.0μg/kg through this method, they are all under DWI drinking waterstandards. This indicates that3-MCPD in environmental water is low and it will nothave a bad effect on human health.(5) According to laboratory Cheng Peng’s extraction methods of free3-MCPDin the oil, then pretreatment of the sample with the optimized conditions andderivative with2-AQ, measured the3-MCPD content in the sample. Results showedthat different brands of peanut oil, soybean oil, rapeseed oil, rice bran oil contents of3-MCPD were50.41μg/kg,33.18μg/kg,61.17μg/kg,157.97μg/kg, due to different oiltype and different oil production process. |
PDF Full Text Request