| Pepper (Piper nigrum),also known as Baichuan, floating pepper and the king pepper,is one kind of the evergreen tropical vine which belongs to pepper Branch (Piperaceae) and Piper (Piper).Pepper is divided into white pepper and black pepper.Fruits are harvested when they become dark green from the late fall to the spring next year. The dried fruit on the condition is named black pepper. fruits are harvested when they become red.Then after flooding the fruit,wiping the pulp and drying the fruit,the fruit on the condition is named white pepper.Pepper originates from India.China first introduced it from Malaysia in 1951, and it was planted experimentally in Qionghai,Hainan.After 1956,a successful introduction is started to try to grow in Guangdong, Yunnan, Guangxi and other provinces.Cultivation area has been expanded to 250 north latitude. Hainan is China's largest province planting pepper,accounting for more than 90% of pepper in China. In 2007,cultivation only in Hainan Province reached 40 million mu with the annual output value exceeding 600 million yuan. Since the favorable climate and geographical environment conditions.Piperine and oil content in our pepar (especially in Hainan) is high, which contents from 5% to 6%, and it has the higher values of smell and taste spicy.Its quality is in the middle and upper level. However, most of our current products are rough from white pepper and black pepper with the low added value.The domestic consumption of the rough products has become saturated, and the deep processing of the pepper is still basically a blank. As the functional role of piperine, both the food industry and the pharmaceutical industry need a higher purity of piperine.The development of high purity, good quality, high yield and low cost of natural piperine products into world market, will help improve China's agricultural economy,conducive to the development of China's pepper industry and improve the economic value of agricultural products and comprehensive utilization.This research mainly focused on the composition of the active ingredient of pepper, piperine extraction and high purity in preparation of the monomer. This system includes the basic components of the composition and pepper aroma composition, organic solvent extraction, ultrasonic extraction, Soxhlet extraction of piperine and pepper oil resin and the use of macroporous resin column method and purified by recrystallization single piperine Body. The thesis experiment forms a complete main chain,"component analysis→extraction→purification→test",which provides the experimental data for industrial mass production. The results are as follows:(1) the composition of the active ingredient of pepperAccording to GB/T 12729,it was determined from Hainan black pepper's and white pepper's water, total ash, insoluble ash, acid insoluble ash, alcohol-insoluble ash, water soluble extract, not volatile ether extract, etc.The results showed that white pepper includes water of 12.54%,total ash of 1.13% insoluble ash of 1.02%,etc.And black pepper includes water of 11.12%, total ash of 3.80%, insoluble ash of 2.03% and so on.Volatile components of pepper was determined by Solid phase micro extraction (SPME), simultaneous distillation extraction (SDE) and steam distillation (DDE). It was found that black and white pepper includes nearly a hundred volatile components.The main aroma includes the a-pinene, 3-carene, D-limonene,4- ethyl-4-methyl-3-(1-isopropenyl-yl)-1-(1-isopropyl)-cyclohexene and so on.(2) pepper oil, pepper oil extraction of the resinPepper essential oil was extracted by Simultaneous distillation and extraction, respectively (SDE) and steam distillation (DDE). Pepper oil resin was extracted by Soxhlet extraction method.Cnditions for extraction of pepper essential oil by Simultaneous distillation extraction (SDE): extraction time of 3h, water ratio of 1:30,fragmentation of 60 mesh.Under these conditions, the yield of white pepper essential oil was up to 1.63%, the yield of black pepper essential oil was up to 1.79%.Conditions for extraction of pepper essential oil of extraction by steam distillation method(DDE):extraction time of 2.5h,water ratio of 1:40, fragmentation of 60 mesh. Under these conditions, the yield of white pepper essential oil was up to 1.49%and the yield of black pepper essential oil was up to1.72%.Conditions for extraction of pepper oil resinby Soxhlet extraction method,:ethanol as solvent,extraction time of 5h,agent ratio of 100:15, fragmentationv of 80 mesh.Under these conditions, the yield of white pepper oleoresin was up to 12.16% and the extraction rate of that was to 98.54%. the yield of Black pepper oleoresin was up to 12.33% and extraction rate of that was to 97.47%.(3) Extraction of piperine and Purification TechnologyConditions for Organic solvent extraction of piperine:95% of ethanol as solvent,2 times of extraction,the extraction time of 2.5h, extraction temperature of 80℃, agent ratio of 4:1,60 mesh of particles. Under these conditions,the yield of white pepper alkali was up to 5.08% and the extraction rate was 97.69%.the yield of black pepper alkali was up to 4.55%, the extraction rate was 96.81%.Ultrasonic extraction (USE) piperine extract which is superior compared with solvent extraction, includes the ethanol concentration of 95%, extraction time of 60min, extraction temperature of 70℃, the soaking time of 2h, dose ratio of 8:1, particles of 60 mesh,2 times of extraction. Under these conditions, the yield of white pepper alkali was up to 5.12% alkali, and the extraction rate was 98.46%.The yield of black pepper alkali was up to 4.61% and the extraction rate was 98.09%.The best technology for purification of piperine needs using of HPD-800 macroporous resin, the column concentration of C= 1.6mg/ML, solution pH value on the columns keeping the same, methanol Analytic solution with pH=3.0,, the column liquid volume of 1.5BV, the column flow rate of 4BV/h and resolution liquid volume of 2.5BV (50mL).Then the organic solvent in analytic solution was evaporated using the rotary evaporator, spin dry matter by analytical solution Material was got.The final purity of piperine in analysis solution liquid was from 44% up to 82%.Spin dry matter in analytical solution Material was Dissolved with 95% ethanol and then cooled crystallization.The piperine monomer with purity of=97% was got.Using Excel data of the curve fitting equations, equation of piperine Macroporous dynamic adsorption by regression analysis is y =3E-06x5-0.0006x4+0.0339x3-0.8695x2+5.7997x+88.726, R2=0.9999; Analytic equation is y=-0.0001x5+0.0039x4-0.0494x3+0.215x2-0.0582x+0.1464, R2= 0.9761.The best conditions for crystallization when purified by recrystallization:recrystallization temperature of 0℃, pH values keeping the same.with 130mg/mL=concentration=230mg/mL,white prismatic crystals of piperine was got.After the pumping of piperine crystals in the first crystallization it appears slightly yellow pigment, with the purity=96%,due to surface attachmentit. White prismatic piperine monomer can be got in the second crystallization with a high purity of= 99%. liquid crystal can continue to concentrate crystallization. The final extraction rate of piperine was above 55%. In the crystallization process, under different crystallization conditions, it has slightly different crystal form respectively, including three kinds needle-like, prismatic and granular.The crystal size was also different. In addition, if the crystallization lasts for 24h at temperature of 5℃at first, and then it crystallized for 24h at temperature of 0℃,there will be a mutual experience of piperine crystalline condensation, and it is more conducive to the separation of crystals and the extraction rate has Increased compared to just using a crystallization temperature. Under these conditions, the initial rate extraction of piperine was up to 32.12%.
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