A passion fruit flavored granule, its preparation method and application

Abstract

This invention discloses a method for preparing passion fruit flavored granules, comprising the following steps: (1) ultrasonic extraction; (2) first low-temperature refrigeration; (3) rotary evaporation concentration; (4) macroporous resin separation; (5) addition of maltodextrin; (6) second low-temperature refrigeration; (7) spray drying; and (8) granulation by sieving. This invention also discloses the passion fruit flavored granules and their application in flavoring and reducing harmful substances in cigarette filters.

Description

Technical Field

[0001] This invention belongs to the field of cigarette production technology, specifically referring to a passion fruit flavored cigarette filter rod flavoring granules, its preparation method, and its application. Background Technology

[0002] The growing conflict between smoking and health has led to tobacco harm reduction and tar reduction becoming an industry trend, and filter rod additives are an effective means of doing so. As a filter rod additive, flavoring granules not only impart a unique aroma to cigarettes and improve smoking quality, but also alter the balance of tar and nicotine, thus reducing tar and harm.

[0003] Passion fruit, also known as granadilla, is a common berry in tropical and subtropical regions, mainly distributed in Yunnan, Guangxi, Taiwan, Fujian, and Hainan provinces of my country. The main cultivated varieties include purple, yellow, hybrid, and variegated types. Passion fruit has a rich aroma and a wide range of aromatic components, including those of strawberries, mangoes, apples, guavas, bananas, and pineapples. Studies have shown that passion fruit contains various aromatic components such as esters, aldehydes, alcohols, and terpenes. Currently, the application of passion fruit in cigarette filter flavoring is a blank area. The preparation of passion fruit filter flavoring granules is of great significance for the utilization of passion fruit aroma components and the development of cigarette filter flavoring granules. Summary of the Invention

[0004] The purpose of this invention is to provide passion fruit flavored granules, their preparation method, and their application in flavoring cigarette filters.

[0005] The technical solution of the present invention is as follows:

[0006] The first aspect of the present invention discloses a method for preparing passion fruit flavored granules, comprising the following steps: (1) ultrasonic extraction; (2) first low-temperature refrigeration; (3) rotary evaporation concentration; (4) macroporous resin separation; (5) addition of maltodextrin; (6) second low-temperature refrigeration; (7) spray drying; and (8) granulation by sieving.

[0007] Preferably, step (1) specifically involves: selecting mature passion fruit to remove passion fruit seeds during pulping and filtration, then adding 97wt% ethanol solution at a mass ratio of material to solvent 1:(5-50), and ultrasonically extracting at room temperature for about 1 hour.

[0008] Preferably, the low-temperature refrigeration conditions in steps (2) and (6) are refrigeration at 2-6℃ for 8-16 hours.

[0009] Preferably, step (3) involves rotary evaporation concentration at 40-50°C to obtain passion fruit extract.

[0010] Preferably, the macroporous resin material used in step (4) is LX-8, and the separation method is as follows: the obtained passion fruit extract is added to the macroporous resin, and eluted with 30wt%, 60wt%, and 90wt% ethanol solutions respectively, and the eluent components are collected.

[0011] Preferably, in step (5), the amount of maltodextrin added is 30 wt%; and it is stirred at 650 r / min for 1 h on a magnetic stirrer, and then homogenized at 16000 rpm for 45 s on a homogenizer.

[0012] Preferably, the spray drying conditions in step (7) are an air inlet temperature of 165°C and a needle working frequency of 10 seconds / cycle.

[0013] Preferably, the sieve in step (8) is 80 mesh.

[0014] The second aspect of this invention discloses passion fruit flavored granules obtained by the preparation method described above.

[0015] The third aspect of this invention discloses the application of the passion fruit flavored granules in adding flavor and reducing harm to cigarette filters.

[0016] The effective effects of this invention are as follows:

[0017] The passion fruit flavoring granules obtained by this invention are loosely structured, uniformly colored yellow powders containing a rich fruity aroma and a scent reminiscent of baked bread. When used as a flavoring agent in cigarette filters, they harmonize with the natural aroma of tobacco, not only improving the smoking quality and purifying the aftertaste, but also imparting a unique sweet and caramelized fragrance, effectively enhancing the flavor. Furthermore, the passion fruit flavoring granules obtained by this invention have a strong adsorption effect on harmful components in cigarette smoke, particularly a significant adsorption effect on hydrocyanic acid. Detailed Implementation

[0018] To make the objectives and technical solutions of this invention clearer, detailed descriptions are provided below in conjunction with specific embodiments. These embodiments are intended to illustrate the content of this invention and not to further limit the scope of protection of this invention. The processes, conditions, reagents, experimental methods, etc., used in the implementation, except as specifically mentioned below, are all common knowledge and general knowledge in the field, and this invention does not impose any particular limitations. Experimental methods in the embodiments that do not specify specific conditions are generally performed under conventional conditions or according to the manufacturer's recommendations. Unless otherwise stated, all technical terms and scientific terms used in this specification have the same meaning as commonly understood by those skilled in the art to which this invention pertains. However, in case of conflict, this specification, including the definitions, shall prevail.

[0019] Example 1: Preparation of passion fruit flavored granules, comprising the following steps:

[0020] Step (1): Select fresh passion fruits that are moderately ripe and have a good appearance and color, and wash them.

[0021] Step (2): Remove the peel from the passion fruit processed in step (1), juice it, filter the seeds, and obtain fruit pulp;

[0022] Step (3): Add 97wt% edible ethanol to the passion fruit pulp treated in step (2) at a material ratio of 1:7.

[0023] Step (4): The passion fruit ethanol extract after step (3) is ultrasonically extracted at room temperature (25℃) for 1 hour;

[0024] Step (5): The passion fruit ethanol extract after step (4) was placed in a 4°C refrigerator for 12 hours and its flavor components were tested. The results are shown in Table 1.

[0025] Step (6): The passion fruit sample solution after step (5) is concentrated by rotary evaporation at 45°C to obtain passion fruit extract.

[0026] Step (7): The passion fruit extract obtained in step (6) was added to LX-8 macroporous resin and eluted with 30wt% ethanol. The eluent components were collected and their flavor components were detected. The results are shown in Table 1.

[0027] Step (8): Add maltodextrin to the 30wt% ethanol eluent obtained in step (7) and make the maltodextrin content 30wt%.

[0028] Step (9): Place the sample obtained in step (8) on a magnetic stirrer and stir at 650 r / min for 1 h, then place it on a homogenizer and homogenize at 16000 rpm for 45 s.

[0029] Step (10): Place the sample obtained in step (9) into a 4°C refrigerator for 12 hours.

[0030] Step (11): The sample obtained in step (10) is spray-dried under the conditions of an air inlet temperature of 165℃ and a needle working frequency of 10 seconds / time.

[0031] Step (12): Pass the sample processed in step (11) through an 80-mesh sieve to obtain passion fruit flavored granules; and evaluate them. The results are shown in Table 2.

[0032] Step (13): Add 0.05% by mass of the flavoring granules obtained in step (12) to each cigarette filter rod. Place the cigarettes with flavoring granules in a constant temperature and humidity chamber (23±1℃) and a relative humidity chamber (60%±2%) for 24 hours to equilibrate. Evaluate the cigarettes obtained. Ordinary cigarettes are used as a blank control (CK). The evaluation results are shown in Table 3. Compare the mainstream smoke components. The results are shown in Table 4.

[0033] Example 2: Preparation of passion fruit flavored granules, comprising the following steps:

[0034] Steps (1)-(6) are the same as in Example 1;

[0035] Step (7): The passion fruit extract obtained in step (6) was added to LX-8 macroporous resin and eluted with 60wt% ethanol. The eluent components were collected and their flavor components were detected. The results are shown in Table 1.

[0036] Steps (8)-(12) are the same as in Example 1;

[0037] Step (13): Add 0.05% by mass of the flavoring granules obtained in step (12) to each cigarette filter rod. Place the cigarettes with flavoring granules in a constant temperature and humidity chamber (23±1℃) and a relative humidity chamber (60%±2%) for 24 hours to equilibrate. Evaluate the cigarettes obtained. Ordinary cigarettes are used as a blank control (CK). The evaluation results are shown in Table 3. Compare the mainstream smoke components. The results are shown in Table 4.

[0038] Example 3: Preparation of passion fruit flavored granules, comprising the following steps:

[0039] Steps (1)-(6) are the same as in Example 1;

[0040] Step (7): The passion fruit extract obtained in step (6) was added to LX-8 macroporous resin and eluted with 90wt% ethanol. The eluent components were collected and their flavor components were detected. The results are shown in Table 1.

[0041] Steps (8)-(12) are the same as in Example 1;

[0042] Step (13): Add 0.05% by mass of the flavoring granules obtained in step (12) to each cigarette filter rod. Place the cigarettes with flavoring granules in a constant temperature and humidity chamber (23±1℃) and a relative humidity chamber (60%±2%) for 24 hours to equilibrate. Evaluate the cigarettes obtained. Ordinary cigarettes are used as a blank control (CK). The evaluation results are shown in Table 3. Compare the mainstream smoke components. The results are shown in Table 4.

[0043] Comparative Example: Same as Example 1, except that the comparative example does not include the rotary evaporation concentration and macroporous resin separation steps. 0.05% by mass of the flavoring granules obtained in step (11) was added to each cigarette filter rod. The cigarettes with the flavoring granules were placed in a constant temperature and humidity chamber (23±1℃) and a relative humidity chamber (60%±2%) for 24 hours to equilibrate. The obtained cigarettes were evaluated, with ordinary cigarettes as the blank control (CK). The evaluation results are shown in Table 3. The mainstream smoke components were compared, and the results are shown in Table 4.

[0044] The methods for detecting flavor components in Table 1 are as follows:

[0045] Absorb 2×10 -5 Add L of passion fruit ethanol extract (or passion fruit ethanol eluent fraction) to the sample vial, then add 1.47 × 10⁻⁶. -3 L of chromatographic acetone was diluted, and finally 1×10⁻⁶ was added. -5 L was prepared as a heptadecane internal standard solution (2 g / L) with anhydrous ethanol, filtered through an organic syringe filter, and then transferred into a chromatographic vial for GC-MS analysis.

[0046] Gas chromatography-mass spectrometry analysis conditions: The capillary column was an Agilent J&W Scientific HP-5ms (30m × 0.25mm × 0.25μm).

[0047] The instrument parameters were set as follows: inlet temperature 250℃, EI ion source temperature 230℃, quadrupole temperature 150℃, high-purity nitrogen (purity greater than 99.999%) as carrier gas, column flow rate 1mL / min, split injection, split ratio 10:1, and injection volume 1×10⁻⁶. -6 L, solvent delay 3 min.

[0048] The temperature ramp-up program was as follows: initial temperature 50℃, maintained for 1 min, ramped up to 200℃ at a rate of 5℃ / min, then ramped up to 260℃ at a rate of 10℃ / min and maintained for 5 min. Mass spectrometry was performed in full scan mode, with a detection range of 35-450 m / z. Continuous sample analysis was conducted in a randomized order to avoid the influence of instrument signal fluctuations.

[0049] The detection methods for mainstream flue gas components in Table 4 are as follows:

[0050] The determination of carbon monoxide in cigarette smoke is based on the national standard GB / T 23355-2009 "Determination of Carbon Monoxide in Gas Phase of Cigarette Smoke - Non-scattering Infrared Method"; the determination of hydrogen cyanide is based on the national standard YC / T 403-2011 "Determination of Hydrogen Cyanide in Mainstream Cigarette Smoke - Ion Chromatography Method"; the determination of phenol is based on the national standard YC / T255-2008 "Determination of Major Phenolic Compounds in Mainstream Cigarette Smoke - High Performance Liquid Chromatography Method"; the determination of benzo[α]pyrene is based on the national standard GB / T 21130-2007 "Determination of Benzo[α]pyrene in Total Particulate Matter of Cigarette Smoke"; and the determination of NNK is based on the national standard YQ / T 17-2012 "Determination of Tobacco-Specific N-Nitrosamines in Total Particulate Matter of Mainstream Cigarette Smoke by High Performance Liquid Chromatography / Tandem Mass Spectrometry"; Ammonia detection refers to National Standard YC / T377-2010 "Determination of Ammonia in Mainstream Cigarette Smoke by Ion Chromatography"; Crotonaldehyde detection refers to National Standard YC / T 254-2008 "Determination of Major Carbonyl Compounds in Mainstream Cigarette Smoke by High Performance Liquid Chromatography".

[0051] Table 1 Flavor components and their content

[0052]

[0053]

[0054]

[0055]

[0056] Table 2 Passion Fruit Flavored Granules

[0057] Color Flavor Organizational Form impurities Example 1 pale yellow A richer fruity aroma Poor fluidity, prone to clumping There are small impurities Example 2 pale yellow A richer fruity aroma Good liquidity, consistent looseness No impurities Example 3 yellow A rich fruity aroma mixed with the scent of toasted bread. Good liquidity, loose and consistent No impurities Comparative Example pale yellow The fruity aroma is rather mild. Poor liquidity, loose and uniform There are small impurities

[0058] Table 3. Cigarette Smoking Evaluation Results

[0059]

[0060] Table 4 Mainstream Smoke Gas Components

[0061]

[0062] As shown in Tables 3 and 4, the passion fruit flavoring granules obtained in Example 3 are the best. They are loosely structured, uniformly colored yellow powders containing a rich fruity aroma and the aroma of baked bread. They also have good flowability and solubility, and are free of visible foreign impurities. Cigarettes with the passion fruit flavoring granules obtained in Example 3 have a better aroma quality and sufficient aroma quantity, better coordination with the natural aroma of tobacco, reduced irritation, and produce a fruity aroma with a rich sweet caramel aroma. At the same time, the reduction effect of harmful components in the mainstream smoke of the cigarette is the most obvious, especially the reduction of hydrocyanic acid in the mainstream smoke.

[0063] The embodiments described are merely preferred embodiments of the present invention and are not intended to limit the invention. Various modifications and variations can be made to the present invention by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.

Claims

1. An application of passion fruit flavored granules for flavoring and reducing harmful substances in cigarette filter rods, characterized in that, The preparation method of passion fruit flavored granules includes the following steps: (1) Select mature passion fruit, pulp it, add 97wt% ethanol solution, and extract it by ultrasonication at room temperature; (2) First low-temperature refrigeration, the low-temperature refrigeration conditions are refrigeration at 4℃ for 12h; (3) Rotary evaporation concentration; (4) Macroporous resin separation; the macroporous resin material used is LX-8, and the separation method is: add the obtained passion fruit extract to the macroporous resin, elute with 90wt% ethanol solution, and collect the eluent components; (5) Add maltodextrin; (6) Second low-temperature refrigeration, the low-temperature refrigeration conditions are refrigeration at 4℃ for 12h; (7) Spray drying; the spray drying conditions are air inlet temperature of 165℃ and needle working frequency of 10 seconds / time; (8) Sieve granulation.

2. The application according to claim 1, characterized in that, Step (3) Rotary evaporation concentration is carried out at 40-50℃ to obtain passion fruit extract.

3. The application according to claim 1, characterized in that, Step (5) The amount of maltodextrin added is 30wt%; and it is stirred at 650r / min for 1h on a magnetic stirrer, and then homogenized at 16000rpm for 45s on a homogenizer.

4. The application according to claim 1, characterized in that, The sieve in step (8) is 80 mesh.

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