The Research Of Dectection And Control Technology For Volatile N-nitrosocompounds In Salted Aquatic Products

Marine food is often as the finest good for its low-fat, high-protein, rich nutrition anddelicious taste. Especially, there is so much accidents occur in food quality and safety,besides the increasingly stringent requirements in international technical barriers, both urgeus to take attach to food safety issues. Among them, the security of marinated aquatic oftenbeen questioned. There have been reports, the high incidence of nasopharyngeal andgastric cancer in the southern coastal places has relationship with long-term consumptionMarinated aquatic. In this topic, we hope to establish a high-sensitivity detection methodfor a variety of nitrosamines in marinated aquatic, specifically the use of high resolutionmass spectrometry technology for peak matching and confirmation to provide an advancedtechnical support to detect the nitrosamines of marinated aquatic. At the same time, theamount of nitrite added, curing temperature, curing time and the different proportion of saltand aquatic are all researched for their impact on the amount of volatile nitrosaminesgenerated in marinated aquatic. There is an important theoretical and practical significanceto investigate these effects and their mutual relations for controlling the nitrosaminescontent of marinated aquatic in actual production process.The main contents and conclusions of the research:1The applied research in detecting the amount of volatile nitrosamines generated formarinated aquatic by gas chromatography/mass spectrometry (GC-MS) technology.A rapid analysis method for the determination of multiple volatile N-nitrosaminescontent in marinated aquatic products is established by gas chromatography/massspectrometry (GC-MS) technology. Six compounds, such asN-nitrosodimethylamine(NDMA),N-diethyl-nitrosamine(NDEA),N-dipropyl-nitrosamines(NDPA),N-nitroso-pyrrolidine(NPYR),N-nitroso-piperidine(NPIP),N-dibutylaminobase nitrosamines (NDBA) have been detected by GC-MS technology. Moreover, we haveoptimized the different extraction methods for sample pre-treatment, different solid-phaseextraction column, and different columns for the separation and detection conditions. Thestudy results show that: the linear correlation coefficient is to0.9998above in the range of10~1000ng/mL; and good reproducibility, the relative standard deviation is less than8%;The recoveries rate up to79%to105%; and own a high sensitivity, low detection limit:besides the detection limit of NDPA is0.03μg/kg, the other five kinds of N-nitrosamines are all0.05μg/kg. By this method, the pre-treatment is simple and fast, the completion of anumber of samples only need2h. For bulk sample analysis detection of N-nitrosaminesmaterial has a good prospect, and easy to operate, so this method is applicable to thedetection of residual content of N-nitrosamines in marinated aquatic.2Study on influence factors of pickled volatile nitrosamines in aquatic productsTake a sea fish for raw materials, through the single factor and the orthogonalexperiment, mainly studies the amount of nitrite added, curing temperature, curing timeand the different proportion of salt and aquatic influence on the volatile nitrosaminescontent in salted fish. The results show that：(1) In the process of salted fish, the amount ofvolatile nitrosamines in salted fish to curing temperature, nitrite added, the differentproportion of salt and aquatic and curing time and other factors.(2) Room temperature25℃, In the process of salted fish, the amount of volatile nitrosamines in salted fish increasesas the pickling time increases, and the amount of N-volatile nitrosamines in the10-12dpickled reach the maximum value. As for the extension of time, N-nitrosamines have littlechanges.(3) Saline product mass ratio was1:4, at room temperature25℃than at low N-content of nitrosamines under the condition of4℃salted fish reached the highest valueappears to be early, and peak value is more higher.(4) Room temperature25℃, thedifferent proportion of salt and aquatic condition pickled, the amount of N-nitrosamineschanges obviously. When the proportion of salt and aquatic is1:8, that the concentration ofsalt is small, N-nitrosamines content is marinated for6hours, it reach the highest,7.8μg/kg;when the proportion of salt and aquatic is1:4,1:2, marinated for10d N-nitrosaminescontent is the highest, respectively is5.8μg/kg,5.3μg/kg, from the show the salt and fishmass ratio increases, the increase of salt concentration, N-nitrosamines content is lower,but with the increase of salt concentration, this trend is relatively small;(5) Be pickled inthe room temperature25℃,with increasing addition of nitrite content, N-nitrosamines arerising in salted fish, within the scope of0~10d,they increase more faster and themaximum peak is very high.(6) According to the results of orthogonal experiment, the saltfish ratio takes greatest influence to N-nitrosamines content the proportion of salt andaquatic, followed by the nitrite added and curing temperature.3Research on the determination and control technology of Aquatic products of volatilenitrosaminesTake sea fish for raw materials，regular checks on the salted fish for content of volatile nitrosamines. Tracking and detection of the results: it is detected a part of the volatilenitrosamines in pickled plum fish, mainly NDMA、NDEA、NDPA、NPYR, with averageconcentration of1.08μg/kg、1.52μg/kg、0.81μg/kg、2.19μg/kg, but did not exceed theGB2762-2005standard limit. In addition, from the theory of experience, combination ofpickled content N-nitrosamines in aquatic product key control technology, were studied bychemical method and biological method to reduce the content of N-nitrosamines aquaticpickled products.