| Diacylglycerol is a natural component in oil,which has the physiological effects of reducing weight,reducing blood fat,and preventing cardiovascular diseases.Diacylglycerol is a safe and harmless new resource for healthy food.Diacylglycerol is widely used in medicine and health,food additives,edible oils and fats,and other fields.At present,the process of commercial DAG is not yet mature,and it is important to explore the production process of diacylglycerol.This study was commissioned by the relevant enterprises,the new domestic liquid lipase LA was used as the enzyme catalyst,the microchannel reactor was used as the reaction device,and the continuous production system of diacylglycerol was built.Optimal reaction conditions for DAG production were obtained by one-factor tests.The DAG production method is amplified in this paper.In this study,quality standards for diacylglycerol were developed,and propose a quality control scheme for key indicators in the production process.The content of 1,3-DAG and fatty acid glycidyl ester(GEs)in the product are tested by high-performance liquid chromatography(HPLC)and gas phase-mass spectrometry(GC-MS)devices to ensure that the quality of the product meets the food hygiene and safety standards.1.Soybean oil and glycerol were used as raw materials,the constant temperature water bath shaker was used as the reaction device,and the catalytic efficiency of the domestic liquid lipases LA,Novozymes 435,and Lipozyme RM IM lipase was compared under the same reaction conditions.The results showed that the reaction was catalyzed by liquid lipase LA most efficiently and better than the remaining two enzymes.Four influencing factors of lipase addition,the molar ratio of soybean oil to glycerol,reaction time,and reaction temperature were explored.Soybean oil: the molar ratio of glycerol is 1:0.8,the amount of enzyme is 2% of the mass of soybean oil,the reaction temperature is 50℃,the reaction time is 2 h,and the content of DAG in the product is 35%.2.The continuous production system of diacylglycerol was built with the microchannel reactor as the reaction device,and the continuous production method of preparing diacylglycerol by enzymatic hydrolysis reaction was explored.Soybean oil and water were used as raw materials,and the influence of four factors of liquid lipase LA concentration and dosage,water feed speed,reaction temperature,and delay tube length on the DAG and TAG content in the product was explored.The optimal reaction conditions were analyzed by univariate: the most suitable concentration of liquid lipase LA was 10000 U/m L;the feed speed ratio of soybean oil,liquid lipase LA and water was 100:3:12 g/min,the reaction temperature was 50℃,and the length of the delay tube was 18 m.Under the optimal process conditions,the DAG content in the product can reach 32%,and the FFA content can be up to34%.3.The continuous production system of diacylglycerol was constructed with the microchannel reactor as the reactor,and the continuous production method of diacylglycerol by enzymatic glycerolysis reaction was explored.The DAG content in the product is affected by four factors: the concentration and dosage of liquid lipase LA,glycerol feeding speed,reaction temperature,and the length of the delay tube.The appropriate preparation method was explored: the most suitable concentration of liquid lipase LA was 10000 U/m L;the feed speed ratio of soybean oil,liquid lipase LA and glycerol was 100:3:8 g/min,the reaction temperature was 50℃,and the length of the delay tube was 18 m.Under optimal process conditions,the DAG content in the product can reach 44%.4.DAG was prepared with soybean oil and glycerol in a shaker.DAG was prepared with soybean oil and water in a microchannel reactor.DAG was prepared with soybean oil and glycerol in a microchannel reactor.These three preparation methods were compared,and the continuous production of diacylglycerol was determined as a better scheme for industrial production: the reaction device was constructed by the constant current pump,micromixer,and delay tube as the main equipment,the glycerolysis reaction was used as the reaction method,and the diacylglycerol was produced with efficient continuity.5.According to the quality provisions of the Ministry of Health Announcement No.18 of 2009 on the new resource food of diacylglycerol edible oil(the content of diacylglycerol as the main index is required to be more than 40%),the quality standard of diacylglycerol is formulated.According to this standard,the key indicators in the production process are determined,and the quality control scheme is proposed.The acyl mobility reaction of1,2-DAG with 1,3-DAG in the product was probed.The ratio of the two isomers 1,2-DAG to1,3-DAG was controlled at 3:7 by thermal conversion.The products were synthesized by the microfluidic continualization device,in which the content of diacylglycerol was 44%.The content of diacylglycerol in the product was 50% after primary molecular distillation.The content of diacylglycerol in the product was 80% after the distillation of secondary molecules.The products were prepared by glycerolysis reaction and Grade I molecular distillation and by Secondary molecular distillation.The content of GEs in these three products was determined by GC-MS,measured at 0.710 mg/kg,1.023 mg/kg,and 5.713mg/kg.The content of GEs was less than 1.0 mg/kg when adsorbed by activated clay-activated carbon.The requirements of the food industry for the content of GEs in oils were met. |
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