Study On Food Quality Safety Analysis And Pollutants Identification Based On Hyphenated Techniques

Food security and food safety rise widely attention in food area, especially for the food safety. In recent years, some safety affairs of food happened now and again, such as artificially and illegally add additives, improper process of raw material and machining, pollution of production and transportation, package material and so on. The feature of these affairs have strong concealment and hardly to be perceived by health supervisor. Food safety are relate to the safety consciousness of producers and some environment factors of production conditions. Meanwhile, effective control method is the key point of all factors in food safety and the most important link is the quality security standard and detection technique of production. Hygienic standard is the basis of food safety judge and detection technique is approach to determining health index quantity. Recently, hygienic standards system of our country falls behind others and the development of detection technique lags behind development of additives and pollutants. Safety hazard substances that possible in food have been found in early stages, and develop sensitive, quick and high-throughput recognition technologies are crucial needs of food hygiene study. Distilled liquors and edible oils are two special foods in people's daily lives. The features of themselves allow most of pollutants dissolved or enriched in it. Process of food production and transportation would bring hidden trouble of safety, such as the fermentation and blending of distilled liquors, process of raw materials and oil extraction, transportation and package materials and so on. This paper take distilled liquors and edible oils as research objects, investigated the production and intermediate links, and food chain of the two materials, analyzed the elements which would influent food safety, determine the corresponding parameters and built sensitive, practical method for analysis and recognition of pollutants, proposed food safety prediction and priority control list. Finally, this paper aimed at offering theory and technology support to the standard formulation and hygiene supervision.Objective: To construct detection and recognition methods for possible components which are not derive from foods. Find out safety hazard substances may in foods, and present conception of pattern recognition technique for food safety and priority control pollutants. Provide methodology and theory basis for food safety pre-warning and hygiene standard formulating.Methods: This paper take distilled liquor and edible oil as study objects. Adopting UPLC/HPLC and GC as means to seperation, combination of derivatization/HS-SPME for sample preparation and UV/FD/MS/MS-MS detectors for detect, establish detection and recognition methods for micro/trace components. By clustering and analog analysis of samples, proposed a pattern recognition technique for food safety. And then obtaine priority control pollutants list of corresponding food.Results:1. Two methods for the determination of four artificial sweeteners, cyclamate, saccharin, acesulfame-K and aspartame in distilled liquor by HPLC-UV and UPLC-MS-MS were established. The concentrations of acesulfame-K and saccharin by HPLC-UV ranging from 1 to 10μg/mL had good linear relationship. The limits of detection (LODs) were 0.16μg/mL and 0.12μg/mL respectively. The average recoveries for them were 92.2% and 96.7%. Aspartame in the range of 10-50μg/mL and cyclamate in the range of 100-1000μg/mL had excellent linearity. LODs of them were 1.24μg/mL and 1.2μg/mL, and the average recoveries for them were 99.3% and 99.2% respectively. The relative standard derivations (RSD) were all within 3%. UPLC-MS-MS method realized simultaneous determination of four sweeteners. The concentrations of them ranging from 10 to 1000μg/L had good linear relationship, and LODs ranging from 0.03 to 0.35μg/L. The average recoveries for them were between 75% and 116%, meanwhile RSD were within 8%. Compared to HPLC-UV, UPLC-MS-MS/MRM method shared the ability to faster and stronger detection and recognition and confirm. The two methods have been used in samples testing, and trace amount of artificial sweeteners in some samples were detected.2. GC-MS were used to develop a method for determination of the main aldehydes in distilled liquor, in the meantime detected total aldehyde by spectrophotometry. Spectrophotometry had good linear relationship between 0.02~0.10mg, while acetaldehyde in the range of 1-100 mg/L and the others each aldehyde were in the range of 1-20 mg/L had good linear relationship by GC-MS. The correlation coefficients between 0.982 to 0.999, and recoveries were 93.9%~114.2% of GC-MS method. The method had good selectivity and hig resolution which suitable to simultaneous analysis of aldehydes in distilled liquor. The two methods have been used in samples testing, and different aldehydes were detected in samples.3. A determination method for Phthalate esters (PAEs) residual in distilled liquor by GC-MS was established. The method possesses good linearity within 0.1-2.0μg/mL (r=0.999). The average recoveries were between 82.8% and 96.5%, and RSD were within 8%, LODs were between 1.7 and 40μg/mL. The method is senstive and reproducible which suitable to monitor of PAEs residual and contamination in distilled liquor. The method was applied to the sample test, and trace amounts of DIBP,DBP,DBEP,DEHP were detected in some samples. Suggest DIBP,DBP,DBEP,DEHP as priority control pollutants.4. A method for the determination of bisphenol A (BPA) residue in polycarbonate (PC) packaging container and its migrant rate in different concentrations of food simulants by HPLC-FD was established. The correlation coefficient of the calibration curve was better (r=0.999) in the range of 0.02 to 4μg/mL. LOD was 10μg/L and the average recovery was between 91% and 108%. RSD was within 6% (n=5). The method was applied to the sample analysis, the content of the two kinds of PC containers were from 17.14 mg/kg to 46.69 mg/kg, and the migrant in the three food simulants were 0.782-1.11 mg/kg, 0.734-0.684 mg/kg and 1.84-2.49 mg/kg respectively. The results suggest PC is not suitable to contacting alcohol-containing food.5. A GC-MS fingerprint building method for distilled liquor and identification technology have been established primarily. The distilled liquor samples were classified according to the results of fingerprint scanning and combination of DPS data processing software. This method can be found abnormal components in distilled liquor and distinguished fermentation/non-fermentation compositions. It can be applicable to identification of distilled liquor.6. A method for determination of five volatile halogenated hydrocarbons in edible oil by HS-SPME-GC-ECD has been established. The limit of detection ranged from 0.02 to 1.4μg/L. The average recovery of the method was between 89% and 105%, and RSD was within 8.5% (n=5). The method is simple and sensitive which suitable to detect trace volatile halogenated hydrocarbons in edible oils.7. A method for simultaneous determination of 35 Volatile Organic Compounds (VOCs) in edible oils was established by HS-SPME-GC-MS. 35 kinds of VOCs in a certain range of concentration has higher linearity and precision. LODs were between 0.03 and 6.84μg/L. The average recovery was between 82.4% and 114%, and RSD was within 13.4%. The method is simple, sensitive and environmental-friendly which suitable to detect trace volatile organic compounds in edible oils. The method was applied to vegetable oil and import and export oil, and some VOCs were detected in samples. The results suggest toluene, ethylbenzene, xylene, hexane, hexanal and chloroform as priority control pollutants; pentane, ethyl acetate and benzaldehyde are potential pollutants possible in edible oils.Conclusion: Sensitive and practical methods for determination of possible hidden substances in distilled liquor and edible oil by combination of different sample pretreatment methods and modern analytical techniques were established, and built a pattern recognition technique for food safety primarily. The methods were applied to actual samples analysis. Suggestions and priority control pollutants list were proposed. These methods are suitable for routine testing analysis. The results can provide methodology and theoretical support for hygiene standard formulating and reference for hygiene supervision.