Method for reducing benzopyrene and plasticizer in capsicum oleoresin and product thereof

Abstract

The invention provides a method for reducing benzopyrene and a plasticizer in capsicum oleoresin and a product thereof. The method specifically comprises the following steps: by taking crude extract ointment of capsicum oleoresin as a raw material, dissolving the crude extract ointment in a small-molecular alcohol solvent, and respectively performing extraction and reverse extraction by CO2 and the small-molecular alcohol solvent in a supercritical two-stage series mode; in an extraction kettle I, CO2 is adopted for extracting the small molecule alcohol solution, and a CO2 extraction phase and a small molecule alcohol phase are obtained; carrying out vacuum concentration and solvent residue removal treatment on the small molecular alcohol phase to obtain capsicum oleoresin with high purity and low benzopyrene and plasticizer; the CO2 extraction phase enters an extraction kettle II and is subjected to reverse extraction with a small-molecule alcohol solvent, and the obtained small-molecule alcohol phase is used for dissolving the capsicum oleoresin crude extraction ointment of the next batch. According to the invention, the removal effect of the plasticizer, benzopyrene and odor in the chili oil extract is effectively improved, so that the benzopyrene, the plasticizer and inherent flavor and odor in the chili oil extract reach extremely low levels, which are obviously superior to those of commercially available products.

Description

Technical Field

[0001] The invention belongs to the technical field of food additive refining, and particularly relates to a method for reducing benzopyrene and plasticizer in capsicum oleoresin and a product thereof. Background Art

[0002] Capsicum oleoresin is a highly spicy oily liquid obtained by extracting and concentrating pepper fruit, which has the inherent flavor and spicy taste of pepper. Its main components are capsaicinoids and capsanthin, which have important functions such as anti-oxidation, antibacterial and anti-tumor. It is mainly used in the production of food additives and seasonings, and is widely used in compound seasonings, puffed foods, and pickled vegetables.

[0003] In recent years, with the rapid development of natural product extraction technology, the production technology of domestic capsicum oleoresin has also been rapidly improved. Domestic capsicum oleoresin has gradually occupied a dominant position in the market, which is mainly reflected in the price advantage.

[0004] However, there are also significant problems with domestic chili oil resin, such as strong grease smell, and excessive benzopyrene and plasticizer content. Among them, after products with strong grease smell are put on the market, their irritation may cause discomfort to consumers. At the same time, when seasoning food, if the smell of chili oil resin is too prominent, it will cover the aroma of other seasonings and affect the overall flavor. Benzopyrene is a polycyclic aromatic hydrocarbon containing benzene rings and is highly carcinogenic. The source of benzopyrene in chili oil resin is mainly due to the high-temperature treatment process in the production process. For example, when extracting and processing chili oil resin, if the temperature is not properly controlled or the processing time is too long, the fat, protein and other components in the pepper may undergo pyrolysis or thermal polymerization at high temperature, thereby forming benzopyrene. In addition, if benzopyrene is contained in the processing equipment or packaging materials, it may also be transferred to the chili oil resin during the processing process. Plasticizers mainly include dibutyl phthalate (DBP) and di(2-ethylhexyl) phthalate (DEHP), both of which are included in the list of Class 2B carcinogens published internationally by the World Health Organization. The sources of DBP and DEHP in chili oil resin mainly include: chili peppers come into contact with materials containing DBP and DEHP during planting, picking, processing or storage, and these substances are fat-soluble and easily remain in chili oil products. At present, the domestic high-content chili oil resin (content>35%) has a benzopyrene content of 80-150μg / kg, DBP of 2-20mg / kg, and DEHP of 15-200mg / kg, which is still a certain distance from the products imported from India.

[0005] At present, the separation and purification methods of chili oil resin reported in the literature mainly include alkali solution treatment method, silica gel column chromatography method, macroporous adsorption resin method, etc. For example, CN201611225649 mentioned that edible oil and low-grade alcohol were used to purify chili oil resin to improve the spiciness of chili oil resin; CN200510013076 mentioned that the chili oil resin was first washed with salt substances and then extracted and refined with a mixed solvent to improve the fluidity and head brightness of the chili oil resin; the article "Preparation of a High-spiciness Chili Oil Resin" mentioned that after the crude extract of chili oil resin was extracted and treated, high-purity chili oil resin could be obtained by column chromatography separation. Although the existing process technologies can meet the requirements of the national standard "GB 28314-2012 Food Safety National Standard Food Additive Chili Oil Resin", the problems of odor, benzopyrene and plasticizer of domestic chili oil resin have not been effectively solved, which has gradually become a bottleneck for the development of the domestic chili oil resin industry.

[0006] In summary, providing a method for reducing benzopyrene and plasticizer in capsicum oleoresin, solving the quality problems still existing in domestic capsicum oleoresin products, and making them more competitive in the market is of great significance to those skilled in the art. Summary of the invention

[0007] The object of the present invention is to provide a method for reducing benzopyrene and plasticizer in capsicum oleoresin. The method comprises the following steps: using the crude oil paste of capsicum oleoresin as raw material, dissolving it with a small molecule alcohol solvent, and obtaining a small molecule alcohol solution of capsicum oleoresin; adopting a supercritical two-stage series mode, extracting and stripping with CO2 and a small molecule alcohol solvent respectively; in an extraction kettle I, extracting the small molecule alcohol solution with CO2, and obtaining a CO2 extraction phase and a raffinate phase (small molecule alcohol phase); after the small molecule alcohol phase is concentrated under reduced pressure and subjected to residual treatment, a high-purity capsicum oleoresin with low benzopyrene and plasticizer is obtained; the CO2 extraction phase enters an extraction kettle II, and stripping is performed with a small molecule alcohol solvent, and the obtained small molecule alcohol phase is used for dissolving the crude oil paste of the next batch of capsicum oleoresin.

[0008] After being processed by the technical scheme provided by the invention, the content of capsaicin in the obtained capsicum oleoresin reaches more than 70%, the average yield is 95.89%, the removal rate of benzopyrene reaches more than 88%, and the removal rates of DBP and DEHP reach more than 93% and 98% respectively.

[0009] To achieve the above object, the present invention provides a method for reducing benzopyrene and plasticizer in capsicum oleoresin, which specifically comprises the following steps:

[0010] (1) using a small molecule alcohol solvent to dissolve the crude extract of capsicum oleoresin to obtain a small molecule alcohol solution of capsicum oleoresin;

[0011] (2) putting the obtained small molecule alcohol solution of capsicum oleoresin into extraction kettle I; and putting a small molecule alcohol solvent into extraction kettle II;

[0012] (3) the capsicum oleoresin small molecule alcohol solution in the extraction kettle 1 is subjected to supercritical CO extraction treatment for a period of time under certain pressure, temperature and flow conditions to obtain the extracted CO phase and small molecule alcohol phase;

[0013] (4) After the CO2 phase in the extraction kettle I enters the extraction kettle II, the small molecule alcohol solvent in the extraction kettle II performs a stripping treatment on the CO2 phase to obtain a stripped small molecule alcohol phase and a CO2 phase, wherein the stripped small molecule alcohol phase is used to dissolve the crude oil paste of the next batch of capsicum oleoresin;

[0014] (5) the small molecule alcohol phase in the extraction kettle I is concentrated under certain temperature and pressure conditions to obtain a refined ointment of pepper extract;

[0015] (6) The obtained pepper extract refined ointment is subjected to certain temperature and pressure conditions to remove the residual solvent, thereby obtaining a high-purity pepper extract ointment.

[0016] In a preferred embodiment, in step (1) and step (2), the small molecule alcohol solvent includes C1-C4 alcohol compounds; preferably, the small molecule alcohol solvent includes one or more of methanol, ethanol and isopropanol; in the present invention, the concentration (volume fraction) of the alcohol compound in the small molecule alcohol solvent is 20-80%.

[0017] In the present invention, the alcohol compounds and their concentrations in the small molecule alcohol solvents in step (1) and step (2) may be the same or different. Preferably, the concentration of the alcohol compounds in the small molecule alcohol solvent used in step (1) is 30 to 80%; and the concentration of the alcohol compounds in the small molecule alcohol solvent used in step (2) is 40 to 60%.

[0018] In a preferred embodiment, in step (1), the mass ratio of the crude capsicum oleoresin paste to the small molecule alcohol solvent is 1:(0.5-10); preferably, the mass ratio of the crude capsicum oleoresin paste to the small molecule alcohol solvent is 1:(2-8).

[0019] In a preferred embodiment, in step (2), the amount of the small molecule alcohol solution of capsicum oleoresin added to the extraction kettle I is 1 / 10 to 1 / 2 of the volume of the extraction kettle; preferably, the amount of the small molecule alcohol solution of capsicum oleoresin added to the extraction kettle I is 1 / 5 to 1 / 2 of the volume of the extraction kettle.

[0020] In a preferred embodiment, in step (2), the amount of the small molecule alcohol solvent added to the extraction kettle II is 1 / 10 to 1 / 2 of the volume of the extraction kettle; preferably, the amount of the small molecule alcohol solvent added to the extraction kettle II is 1 / 5 to 1 / 2 of the volume of the extraction kettle.

[0021] In a preferred embodiment, in step (3), the supercritical extraction conditions of the small molecule alcohol solution of capsicum oleoresin in the extraction kettle I are: extraction pressure of 10-20Mpa; extraction temperature of 40-60°C; extraction flow rate of 5-20 times the volume of the liquid to be extracted / h, and extraction time of 2-8h; preferably, the supercritical extraction conditions of the small molecule alcohol solution of capsicum oleoresin in the extraction kettle I are: pressure of 12-18Mpa; extraction temperature of 40-55°C; extraction flow rate of 8-20 times the volume of the liquid to be extracted / h.

[0022] In a preferred embodiment, in step (4), the back-extraction conditions of the CO2 phase in the extraction kettle II are: extraction pressure 10-20Mpa; extraction temperature 40-60°C; extraction flow rate 5-20 times the volume of the liquid to be extracted / h, and extraction time 2-8h; preferably, the back-extraction conditions of the CO2 phase in the extraction kettle II are: extraction pressure 12-18Mpa; extraction temperature 40-55°C; extraction flow rate 8-20 times the volume of the liquid to be extracted / h.

[0023] In a preferred embodiment, in step (4), after the stripping is completed, the pressure of the separation device I is 6-8 MPa and the temperature is 40-50°C; the pressure of the separation device II is 4-6 MPa and the temperature is 40-50°C.

[0024] In a preferred embodiment, in step (5), the conditions for concentrating the small molecule alcohol phase in the extraction kettle I are: a concentration temperature of 40 to 90° C. and a concentration pressure of -0.02 to -0.08 MPa.

[0025] In a preferred embodiment, in step (6), the conditions for desolventizing the pepper extract refined oil paste are: the concentration temperature is 60 to 100°C, and the desolventizing pressure is -0.06 to -0.09Mpa. Preferably, the conditions for desolventizing the pepper extract refined oil paste are: the desolventizing temperature is 70 to 90°C, and the desolventizing pressure is -0.07 to -0.09Mpa.

[0026] In the present invention, the purpose of concentrating the small molecule alcohol phase in the extraction kettle I is to recover the solvent from the solution containing obvious solvent to obtain a concentrated ointment; the purpose of desolventizing the refined ointment of the pepper extract is to further remove the solvent from the concentrated ointment containing trace solvents so that the residual solvent reaches an extremely low level. Based on the above purpose, the reaction temperature and pressure of the concentration step in the present invention are designed to be relatively low, which is conducive to maintaining the active ingredients, while the desolventizing temperature and pressure are relatively high, which is conducive to improving the desolventizing efficiency.

[0027] In a preferred embodiment, in step (6), the capsaicin content in the prepared high-purity pepper extract ointment reaches more than 70%, the average yield is 95.89%, the removal rate of benzopyrene reaches more than 88%, and the removal rates of DBP and DEHP reach more than 93% and 98% respectively.

[0028] Another object of the present invention is to provide a capsicum oleoresin prepared by any of the above methods for reducing benzopyrene and plasticizer in capsicum oleoresin. The capsicum oleoresin is mixed with edible oils and fats to form a capsicum oleoresin with a mass concentration of 10%, wherein the average benzopyrene content is ≤10 μg / kg, the DBP content is ≤0.3 mg / kg, the DEHP content is ≤1.5 mg / kg, and there is no obvious pepper smell.

[0029] In a preferred embodiment, the edible oil includes one or more of soybean oil, sunflower oil, and rapeseed oil.

[0030] Compared with the prior art, the technical solution of the present invention has the following advantages:

[0031] In the present invention, a crude capsicum oleoresin extract is firstly dissolved in a specific ratio by using a small molecule alcohol, and then the crude capsicum oleoresin extract alcohol solution in an extraction kettle I is extracted by using CO2 in a supercritical two-stage series mode, so that not only the fat-soluble impurities in the crude extract and capsaicin can be effectively separated, but also the odor, benzopyrene and plasticizer therein can be removed at the same time, so as to obtain a capsicum oleoresin product with high content, low odor, low benzopyrene and plasticizer; and the CO2 phase after the first extraction is stripped by the small molecule alcohol in the extraction kettle II, so that part of the capsaicin entrained therein can be recovered into the small molecule alcohol phase, and then the small molecule alcohol phase is used for the dissolution of the crude capsicum oleoresin extract, thereby significantly improving the refined yield of the capsicum oleoresin.

[0032] Through the technical scheme of the present invention, not only the content of capsicum oleoresin is effectively increased, the fluidity and state of the low-content product are improved, but also the levels of capsicum odor, benzopyrene and plasticizer are reduced, and the comprehensive quality of the capsicum oleoresin product is improved; moreover, the adopted process conditions are environmentally friendly and green, suitable for industrial production, and provide a reference for the industrial development of capsicum oleoresin. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] These and / or other aspects and advantages of the present invention will become more clear and easier to understand from the following detailed description of the embodiments of the present invention in conjunction with the accompanying drawings, in which:

[0034] Figure 1 It is a process flow chart of the present invention. DETAILED DESCRIPTION

[0035] In order to enable those skilled in the art to better understand the present invention, the present invention is further described in detail below in conjunction with the accompanying drawings and specific implementation methods, but it should be understood that the protection scope of the present invention is not limited to the specific implementation methods.

[0036] The embodiment of the present invention solves the problems that the capsicum oleoresin prepared by the prior art has a strong odor and high content of benzopyrene and plasticizer, by providing a method for reducing benzopyrene and plasticizer in capsicum oleoresin and a product thereof.

[0037] The technical solution of the present application is described in detail below through specific embodiments:

[0038] If not otherwise specified, the technical means used in the present invention are conventional means well known to those skilled in the art, and the various raw materials, reagents, instruments and equipment used in the present invention can be purchased from the market or prepared by existing methods. The reagents used in the present invention are analytically pure unless otherwise specified. The crude extract of capsicum oleoresin used in the embodiments of the present invention is the crude extract of capsicum oleoresin produced by Henan Zhongda Hengyuan Biotechnology Co., Ltd.

[0039] The method used for detecting the benzopyrene content in the present invention is the determination of benzo(α)pyrene in food according to GB 5009.27-2016 National Food Safety Standard; the method used for detecting the DBP and DEHP contents is the determination of phthalates in food according to GB 5009.271-2016 National Food Safety Standard.

[0040] Example 1

[0041] a) taking 10 kg of crude extract of capsicum oleoresin (capsaicin content of 32.18%; benzopyrene content of 87.66 μg / kg; DBP content of 2.84 mg / kg, DEHP content of 82.64 mg / kg), adding 30 kg of 75% methanol, stirring and mixing at room temperature to obtain a small molecule alcohol solution of capsicum oleoresin;

[0042] b) The small molecule alcohol solution of capsicum oleoresin is put into extraction kettle I, and 30kg75% methanol is put into extraction kettle II. The extraction pressure of extraction kettle I and extraction kettle II is 15Mpa, and the extraction temperature is 45°C; the pressure of separation I is 8Mpa, and the temperature of separation I is 40°C; the pressure of separation II is 4Mpa, and the temperature of separation II is 40°C; the extraction is started for 4h under the condition of extraction flow rate of 300-320L / h, and the capsicum oleoresin raffinate (small molecule alcohol phase) of extraction kettle I and the small molecule alcohol stripping liquid of extraction kettle II are obtained.

[0043] c) The capsicum oleoresin raffinate of extraction kettle I is concentrated to a solvent residual amount of <1% at 75-80° C. and -0.07-0.09 MPa to obtain a refined capsicum extract ointment; the small molecule alcohol stripping solution of extraction kettle II is used for dissolving the next batch of capsicum oleoresin crude extract.

[0044] d) The pepper extract refined ointment is subjected to a desolventizing treatment at 80-90° C. and -0.07-0.09 MPa to obtain 4.24 kg of a high-purity pepper extract ointment product with a capsaicin content of 73.12%, a benzopyrene content of 28.83 μg / kg, a DBP content of 0.51 mg / kg, and a DEHP content of 2.48 mg / kg; the product has no obvious pepper smell residue.

[0045] Example 2

[0046] a) taking 6 kg of crude extract of capsicum oleoresin (capsaicin content of 35.75%; benzopyrene content of 105.42 μg / kg; DBP content of 4.16 mg / kg, DEHP separation of 64.25 mg / kg), adding 12 kg of 70% methanol, stirring and mixing at room temperature to obtain a small molecule alcohol solution of capsicum oleoresin;

[0047] b) The small molecule alcohol solution of capsicum oleoresin is put into extraction kettle I, and 20kg70% methanol is put into extraction kettle II. The extraction pressure of extraction kettle I and extraction kettle II is 18Mpa, and the extraction temperature is 40°C; the pressure of separation I is 8Mpa, and the temperature of separation I is 40°C; the pressure of separation II is 4Mpa, and the temperature of separation II is 40°C; extraction is started for 3h under the condition of extraction flow rate of 350-380L / h, and the capsicum oleoresin raffinate (small molecule alcohol phase) of extraction kettle I and the small molecule alcohol stripping solution of extraction kettle II are obtained.

[0048] c) The capsicum oleoresin raffinate of extraction kettle I is concentrated to a solvent residual content of <1% at 82-87° C. and -0.06--0.08 MPa to obtain a refined pepper extract ointment; the small molecule alcohol stripping solution of extraction kettle II is used to dissolve the next batch of capsicum oleoresin crude extract.

[0049] d) The refined pepper extract ointment is subjected to a desolventizing treatment at 78 to 88° C. and -0.07 to -0.09 MPa to obtain 2.67 kg of a high-purity pepper extract ointment product with a capsaicin content of 75.86%, a benzopyrene content of 25.37 μg / kg, a DBP content of 0.38 mg / kg, and a DEHP content of 1.64 mg / kg; the product has no obvious pepper smell residue.

[0050] Example 3

[0051] a) taking 6 kg of crude extract of capsicum oleoresin (capsaicin content of 30.87%; benzopyrene content of 118.33 μg / kg; DBP content of 2.97 mg / kg, DEHP content of 40.17 mg / kg), adding 20 kg of 70% ethanol, stirring and mixing at room temperature to obtain a small molecule alcohol solution of capsicum oleoresin;

[0052] b) The small molecule alcohol solution of capsicum oleoresin is put into extraction kettle I, and 20kg70% ethanol is put into extraction kettle II. Extraction kettle I and extraction kettle II have an extraction pressure of 12Mpa and an extraction temperature of 50°C; separation I has a pressure of 8Mpa and a temperature of 40°C; separation II has a pressure of 4Mpa and a temperature of 40°C; extraction begins for 3.5h under the condition of an extraction flow rate of 380-400L / h to obtain the capsicum oleoresin raffinate (small molecule alcohol phase) of extraction kettle I and the small molecule alcohol stripping solution of extraction kettle II.

[0053] c) The capsicum oleoresin raffinate of extraction kettle I is concentrated to a solvent residual amount of <1% at 80-85° C. and -0.06--0.08 MPa to obtain a refined pepper extract ointment; the small molecule alcohol stripping solution of extraction kettle II is used for dissolving the next batch of capsicum oleoresin crude extract.

[0054] d) The refined pepper extract ointment is subjected to a desolventizing treatment at 80-90° C. and -0.07-0.09 MPa to obtain 2.47 kg of a high-purity pepper extract ointment product with a capsaicin content of 71.48%, a benzopyrene content of 31.44 μg / kg, a DBP content of 0.60 mg / kg, and a DEHP content of 2.87 mg / kg; the product has no obvious pepper smell residue.

[0055] Comparative Example 1

[0056] a) Take 10kg of crude extract of capsicum oleoresin (capsaicin content is 32.18%; benzopyrene content is 87.66μg / kg; DBP content is 2.84mg / kg, DEHP content is 82.64mg / kg) and directly put into extraction kettle, extraction pressure is 12Mpa, extraction temperature is 50℃; separation I pressure is 8Mpa, separation I temperature is 40℃; separation II pressure is 4Mpa, separation II temperature is 40℃; extraction is started under extraction flow rate 380~400L / h condition for 3.5h, and obtain capsicum oleoresin raffinate (small molecule alcohol phase) of extraction kettle.

[0057] b) the capsicum oleoresin raffinate is subjected to a desolventizing treatment at 80-90° C. and -0.07-0.09 MPa to obtain 5.56 kg of a highly purified capsicum oleoresin product having a capsaicin content of 45.87%, a benzopyrene content of 76.42 μg / kg, a DBP content of 2.06 mg / kg, and a DEHP content of 67.41 mg / kg; and the product has no obvious pepper odor residue.

[0058] Comparative Example 2

[0059] a) 10 kg of crude capsicum oleoresin extract (capsaicin content of 32.18%; benzopyrene content of 87.66 μg / kg; DBP content of 2.84 mg / kg, DEHP content of 82.64 mg / kg) was added, 40 kg of 70% ethanol was added and stirred at 50° C. for 30 min to obtain a small molecule alcohol solution of capsicum oleoresin.

[0060] b) standing the small molecule alcohol solution of capsicum oleoresin at 50° C. for 1 h to separate, slowly releasing the lower alcohol phase, extracting the upper layer 4 times in the same manner as in a), combining the lower layer solutions to obtain a refined capsicum oleoresin solution;

[0061] c) concentrating the capsicum oleoresin refined liquid at 75-80° C. and -0.07-0.09 MPa to a solvent residual content of <1% to obtain a capsicum extract refined ointment.

[0062] d) The refined pepper extract ointment is subjected to a desolventizing treatment at 80-90° C. and -0.07-0.09 MPa to obtain 7.20 kg of a pepper extract ointment product with a high purity, a capsaicin content of 41.92%, a benzopyrene content of 78.34 μg / kg, a DBP content of 3.17 mg / kg, and a DEHP content of 79.68 mg / kg; the product has a more obvious pepper smell.

[0063] Application Example 1

[0064] The pepper extract ointments prepared in Examples 1 to 3 and Comparative Examples 1 to 2 were analyzed and tested, and the results are shown in Table 1.

[0065] Table 1

[0066]

[0067]

[0068] According to the results in Table 1, we can see that:

[0069] (1) The capsaicin content of the embodiment is 71.48-75.86%, and the average content is 72.30%, which is 57.61% higher than that of Comparative Example 1 and 72.47% higher than that of Comparative Example 2; the refining yield of the embodiment is 94.26-96.28%, and the average content is 95.89%, which is 21.01% higher than that of Comparative Example 1 and 2.26% higher than that of Comparative Example 2;

[0070] (2) The refined capsicum oleoresin of the embodiment has no obvious pepper smell; the refined capsicum oleoresin of Comparative Example 1 has no obvious pepper smell; the refined capsicum oleoresin of Comparative Example 2 has obvious pepper smell.

[0071] (3) The benzopyrene content of the embodiment is 28.83-31.44 μg / kg, the removal rate is 86.06-89.31%, and the average removal rate of benzopyrene is 88.14%; compared with Comparative Example 1, it is increased by 0.71 times, and compared with Comparative Example 2, it is increased by 1.47 times;

[0072] (4) The plasticizer DBP content of the embodiment is 0.38-0.60 mg / kg, the removal rate is 91.67-95.94%, and the average DBP removal rate is 93.33%, which is 0.56 times higher than that of Comparative Example 1 and 3.75 times higher than that of Comparative Example 2; the plasticizer DEHP content is 1.64-2.87 mg / kg, the removal rate is 97.05-98.87%, and the average DEHP removal rate is 98.22%, which is 0.80 times higher than that of Comparative Example 1 and 2.21 times higher than that of Comparative Example 2;

[0073] Application Example 2

[0074] The pepper extract ointment products prepared in Examples 1 to 3 and Comparative Examples 1 to 2 were added with soybean oil, respectively, to prepare pepper oleoresin products with a mass concentration of 6.6% and 10%, and analyzed and tested. The results are shown in Table 2.

[0075] Table 2

[0076]

[0077]

[0078] According to the results in Table 2, we can see that:

[0079] (1) The benzopyrene contents of the prepared 6.6% and 10% capsicum oleoresin in the embodiment are 2.24-3.02 μg / kg and 3.46-4.55 μg / kg, respectively, both of which meet the requirement of ≤10 μg / kg; the benzopyrene contents of the prepared 6.6% and 10% capsicum oleoresin in Comparative Example 1 are 11.48 μg / kg and 17.21 μg / kg, respectively, and the benzopyrene contents of the prepared 6.6% and 10% capsicum oleoresin in Comparative Example 2 are 13.82 μg / kg and 18.94 μg / kg, both of which do not meet the requirement of ≤10 μg / kg;

[0080] (2) The DBP contents of the corresponding plasticizers in the embodiment of the invention are 0.05-0.07 mg / kg and 0.06-0.11 mg / kg, respectively, for 6.6% and 10% capsicum oleoresin, both of which meet the requirement of ≤0.3 mg / kg; the DBP contents of the plasticizers in Comparative Example 1 of 6.6% and 10% capsicum oleoresin are 0.34 mg / kg and 0.48 mg / kg, respectively, and the DBP contents of the plasticizers in Comparative Example 2 of 6.6% and 10% capsicum oleoresin are 0.52 mg / kg and 0.77 mg / kg, respectively, both of which do not meet the requirement of ≤0.3 mg / kg;

[0081] (3) The DEHP contents of the plasticizers corresponding to the prepared 6.6% and 10% capsicum oleoresin in the embodiment are 0.20-0.28 mg / kg and 0.28-0.44 mg / kg, respectively, both of which meet the requirement of ≤1.50 mg / kg; the DEHP contents of the plasticizers corresponding to the prepared 6.6% and 10% capsicum oleoresin in Comparative Example 1 are 9.84 mg / kg and 15.76 mg / kg, respectively, and the DEHP contents of the plasticizers corresponding to the prepared 6.6% and 10% capsicum oleoresin in Comparative Example 2 are 12.60 mg / kg and 21.47 mg / kg, respectively, both of which fail to meet the requirement of ≤1.50 mg / kg.

[0082] In summary, in view of the quality problems of high benzopyrene and plasticizer content in chili products in the prior art, the present invention uses supercritical CO2 as a solvent for the first time, and adopts a two-stage series extraction of a small molecule alcohol solution of a crude extract of chili oleoresin by means of a first-stage extraction and a second-stage stripping method. After the raffinate is concentrated and desolventized, a chili oleoresin with a content of more than 70% is obtained, and the average yield is 95.89%. The removal rate of benzopyrene reaches more than 88%, and the removal rates of DBP and DEHP reach more than 93% and 98% respectively. The chili oleoresin prepared with 10% benzopyrene can meet the requirements of ≤10μg / kg, DBP≤0.3mg / kg, and DEHP≤1.5mg / kg, and has no obvious chili smell.

[0083] Compared with the products produced by the traditional process, the production process of the present invention has obvious advantages in improving the content and yield of the refined product of capsicum oleoresin, and removing odor, benzopyrene and plasticizer. At the same time, the capsicum oleoresin produced by the present invention can be applied to the formulation of oil-soluble and water-soluble products, and its quality not only meets the requirements of food application, but also can significantly improve the safety indicators such as benzopyrene and plasticizer, which is significantly better than the products produced by the traditional process conditions.

[0084] The foregoing description of specific exemplary embodiments of the present invention is for the purpose of illustration and demonstration. These descriptions are not intended to limit the present invention to the precise form disclosed, and it is clear that many changes and variations can be made based on the above teachings. The purpose of selecting and describing the exemplary embodiments is to explain the specific principles of the present invention and its practical application, so that those skilled in the art can realize and utilize various different exemplary embodiments of the present invention and various different selections and changes. The scope of the present invention is intended to be limited by the claims and their equivalents.

Claims

1. A method for reducing benzopyrene and plasticizer in capsicum oleoresin, characterized in that: The following steps are involved: The crude oil paste of capsicum oleoresin is used as raw material, and after dissolving with a small molecule alcohol solvent, a small molecule alcohol solution of capsicum oleoresin is obtained; a supercritical two-stage series mode is adopted, and CO2 and a small molecule alcohol solvent are used for extraction and back-extraction respectively; the small molecule alcohol phase obtained by extraction is concentrated under reduced pressure and desolventized to obtain high-purity capsicum oleoresin with low benzopyrene and plasticizer; the small molecule alcohol phase obtained by back-extraction is used to dissolve the next batch of crude oil paste of capsicum oleoresin.

2. The method for reducing benzopyrene and plasticizer in capsicum oleoresin as claimed in claim 1, characterized in that: The specific steps include: (1) using a small molecule alcohol solvent to dissolve the crude extract of capsicum oleoresin to obtain a small molecule alcohol solution of capsicum oleoresin; (2) putting the obtained small molecule alcohol solution of capsicum oleoresin into extraction kettle I; and putting a small molecule alcohol solvent into extraction kettle II; (3) the capsicum oleoresin small molecule alcohol solution in the extraction kettle 1 is subjected to supercritical CO extraction treatment for a period of time under certain pressure, temperature and flow conditions to obtain the extracted CO phase and small molecule alcohol phase; (4) After the CO2 phase in the extraction kettle I enters the extraction kettle II, the small molecule alcohol solvent in the extraction kettle II performs a stripping treatment on the CO2 phase to obtain a stripped small molecule alcohol phase and a CO2 phase, wherein the stripped small molecule alcohol phase is used to dissolve the crude oil paste of the next batch of capsicum oleoresin; (5) the small molecule alcohol phase in the extraction kettle I is concentrated under certain temperature and pressure conditions to obtain a refined ointment of pepper extract; (6) The obtained pepper extract refined ointment is subjected to certain temperature and pressure conditions to remove the residual solvent, thereby obtaining a high-purity pepper extract ointment.

3. The method for reducing benzopyrene and plasticizer in capsicum oleoresin as claimed in claim 2, characterized in that: In step (1) and step (2), the small molecule alcohol solvent includes C1-C4 alcohol compounds.

4. The method for reducing benzopyrene and plasticizer in capsicum oleoresin as claimed in claim 1, characterized in that: In step (1), the mass ratio of the crude capsicum oleoresin extract to the small molecule alcohol solvent is 1:(0.5-10).

5. The method for reducing benzopyrene and plasticizer in capsicum oleoresin as claimed in claim 1, characterized in that: In step (3), the supercritical extraction conditions of the small molecule alcohol solution of capsicum oleoresin in the extraction kettle I are as follows: extraction pressure is 10-20Mpa; extraction temperature is 40-60°C; extraction flow rate is 5-20 times / h of the volume of the liquid to be extracted, and extraction time is 2-8h.

6. The method for reducing benzopyrene and plasticizer in capsicum oleoresin as claimed in claim 1, characterized in that: In step (4), the back extraction conditions of the CO2 phase in the extraction kettle II are: extraction pressure 10-20Mpa; extraction temperature 40-60°C; extraction flow rate 5-20 times the volume of the extract / h, and extraction time 2-8h.

7. The method for reducing benzopyrene and plasticizer in capsicum oleoresin as claimed in claim 1, characterized in that: In step (5), the conditions for concentrating the small molecule alcohol phase in the extraction kettle I are: a concentration temperature of 40 to 90° C. and a concentration pressure of -0.02 to -0.08 MPa; In step (6), the conditions for desolventizing the pepper extract refined ointment are: the desolventizing temperature is 60 to 100° C., and the desolventizing pressure is -0.06 to -0.09 MPa.

8. The method for reducing benzopyrene and plasticizer in capsicum oleoresin as claimed in claim 1, characterized in that: In step (6), the capsaicin content in the prepared high-purity pepper extract ointment reaches more than 70%, the average yield is 95.89%, the removal rate of benzopyrene reaches more than 88%, and the removal rates of DBP and DEHP reach more than 93% and 98% respectively.

9. The capsicum oleoresin prepared by the method for reducing benzopyrene and plasticizer in capsicum oleoresin as claimed in any one of claims 1 to 8.

10. Capsicum oleoresin as claimed in claim 9, characterized in that The capsicum oleoresin is prepared with edible oils and fats into a 10% concentration of capsicum oleoresin, the average benzopyrene content of which is ≤10 μg / kg, the DBP content is ≤0.3 mg / kg, the DEHP content is ≤1.5 mg / kg, and there is no obvious pepper smell.

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