CN111454768B - Preparation method and application of garlic seedling volatile oil - Google Patents

Preparation method and application of garlic seedling volatile oil Download PDF

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CN111454768B
CN111454768B CN202010289626.4A CN202010289626A CN111454768B CN 111454768 B CN111454768 B CN 111454768B CN 202010289626 A CN202010289626 A CN 202010289626A CN 111454768 B CN111454768 B CN 111454768B
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garlic
volatile oil
oil
seedling
yellow
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CN111454768A (en
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张扬
虞晓瑾
徐海
杨贵洪
孔云琪
王高超
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Jinzun Technology Development (Chongqing) Co.,Ltd.
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Changshu Institute of Technology
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    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/44—Oils, fats or waxes according to two or more groups of A61K47/02-A61K47/42; Natural or modified natural oils, fats or waxes, e.g. castor oil, polyethoxylated castor oil, montan wax, lignite, shellac, rosin, beeswax or lanolin
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Abstract

The invention provides a preparation method of garlic seedling volatile oil and an anticoagulant product application thereof. Microwave/ultrasonic wave assisted extraction of garlic oil seedling volatile oil, wherein the process conditions are as follows: the feed-liquid ratio of garlic seedlings to distilled water is 1:30, the microwave-assisted extraction power is 600W, the microwave-assisted extraction time is 10min, the ultrasonic-assisted extraction power is 70W, and the ultrasonic-assisted extraction time is 25 min. Under the condition, the extraction rates of the volatile oil of the two garlic seedlings (garlic sprouts and garlic yellow) are respectively 0.55 +/-0.02% and 0.78 +/-0.06%. The analysis result of gas chromatography-mass spectrometry is further proved by adopting an infrared spectrum coupling second derivative infrared technology. The two garlic seedling volatile oils have obvious anticoagulation effect, can activate endogenous, exogenous and common coagulation ways and reduce the fibrinogen content, and can be prepared into anticoagulation functional soft capsules.

Description

Preparation method and application of garlic seedling volatile oil
Technical Field
The invention belongs to the field of preparation and application of natural products, and particularly relates to a preparation method of garlic seedling volatile oil and application of the garlic seedling volatile oil in anticoagulation.
Background
Cardiovascular diseases (CVD) are the most fatal diseases worldwide. In China, about 2.9 hundred million CVD patients have higher death rate than malignant tumors, and account for more than 40 percent of death components of diseases. Thrombus is the "extreme" of CVD, and imbalance between blood coagulation and anticoagulation can cause hypercoagulability of blood to induce thrombus, thereby accelerating the CVD process. Therefore, anticoagulation is the basis and key for CVD control. Heparin (Heparin) and derivatives thereof are the most widely used anticoagulant drugs in clinical application at present, and although the Heparin and derivatives thereof play an important role in preventing and treating CVD, complications of bleeding caused by excessive anticoagulation cannot be overcome all the time. In addition, heparin belongs to animal origin polysaccharides, which also increases the risk of infection by animal pathogens. Therefore, the search for a "highly effective and low-toxicity" heparin substitute has become one of the most concerned problems in the fields of medicine and functional food.
The garlic sprout is seedling of garlic of Allium of Liliaceae, and is obtained by placing garlic clove in container for water culture. The garlic sprouts are delicious in taste, strong in garlic flavor and short in growth period, can be picked once in two or three days, are popular with people and are common and delicious on a dining table. Garlic yellow is another young seedling of garlic, and is a vegetable obtained by cultivating garlic cloves in dark conditions by softening. Compared with garlic sprouts, the garlic yellow has softer texture, light yellow color and stronger garlic flavor, and is also widely popular among people. The functional factors and health care function of garlic have been widely proved and applied, and the two garlic seedlings which are also eaten as vegetables are reported. Although the garlic sprouts and the blanched garlic are derived from garlic, the active ingredients and the functions of the garlic sprouts are different due to the difference of metabolic organs of different parts of plants, and the functional factors and the health care functions of the two garlic sprouts are required to be explored, so that the comprehensive development and utilization of garlic-derived vegetables are promoted, and the added value of agricultural products is improved.
Disclosure of Invention
The invention aims to provide a preparation method of garlic seedling volatile oil and an anticoagulant product application thereof.
According to the first aspect of the invention, the invention provides a preparation method of volatile oil of garlic sprouts, which takes fresh garlic sprouts and blanched garlic as raw materials and adopts a microwave/ultrasonic wave assisted steam distillation method to respectively prepare the volatile oil of the garlic sprouts and the blanched garlic blanched.
The preparation method of the garlic seedling volatile oil specifically comprises the following steps:
weighing a certain amount of fresh garlic sprouts and/or garlic yellow, cutting into small sections of 1-2 cm, placing the small sections into a volatile oil extraction device, and soaking the small sections in distilled water for 2 hours according to a certain material-liquid ratio; placing the volatile oil extraction device in an ultrasonic-microwave synergistic extraction instrument, refluxing at 100-105 ℃, adjusting to a certain microwave power, and extracting for a certain time; switching to an ultrasonic mode, adjusting to a certain ultrasonic power, and extracting for a certain time; cooling, collecting volatile oil layer, collecting water layer, further enriching volatile oil with dichloromethane as solvent, evaporating at low temperature under reduced pressure to remove solvent, and mixing oil layers to obtain garlic sprout and/or garlic yellow volatile oil respectively.
Preferably, the feed-liquid ratio of the fresh garlic sprouts and/or the garlic yellow to the distilled water is 1: 20-1: 50; further preferably 1: 30;
preferably, the microwave-assisted extraction power is 400W-800W, and more preferably 600W;
preferably, the microwave-assisted extraction time is 5min to 20min, and further preferably 10 min;
preferably, the ultrasonic auxiliary extraction power is 50W-100W, and more preferably 70W;
preferably, the ultrasonic-assisted extraction time is 10min to 40min, and further preferably 25 min;
preferably, the feed-liquid ratio of the fresh garlic sprouts or the garlic cloves to the distilled water is 1:30, the microwave-assisted extraction power is 600W, the microwave-assisted extraction time is 10min, the ultrasonic-assisted extraction power is 70W, and the ultrasonic-assisted extraction time is 25 min. Under the condition, the extraction rates of the volatile oil of the garlic sprout and the garlic clove yellow are respectively 0.55 +/-0.02% and 0.78 +/-0.06%.
Preferably, the main component of the volatile oil of garlic sprout and/or the volatile oil of garlic yellow is a sulfur-containing compound; the sulfur-containing compounds include diallyl disulfide, diallyl trisulfide and diallyl tetrasulfide. 16 and 14 volatile compounds are respectively identified from the volatile oil of garlic sprouts and garlic yellow. Wherein the sulfur-containing compound is the main component and respectively accounts for 87.18% and 94.40% of the volatile oil of garlic sprout and garlic clove; diallyl disulfide is the most abundant compound (42.10% of volatile oil of garlic sprout and 45.13% of volatile oil of garlic clove); then diallyl trisulfide (accounting for 25.49% of the volatile oil of the garlic sprouts and 31.88% of the volatile oil of the garlic leaves) and diallyl tetrasulfide (accounting for 6.25% of the volatile oil of the garlic sprouts and 8.23% of the volatile oil of the garlic leaves) are added.
According to the second object of the invention, the invention provides a method for identifying garlic seedling volatile oil by infrared spectrum coupling second derivative infrared technology; the volatile oil of garlic sprout comprises any one of volatile oil of garlic sprout or volatile oil of garlic yellow; the method comprises the following specific steps:
loading the dried potassium bromide solid powder into a tablet machine, and pressing into potassium bromide tablets with certain specifications; uniformly coating a certain amount of garlic seedling volatile oil on the surface of a potassium bromide tablet; placing in an infrared spectrometer, scanning within a certain wave number range, and drawing an infrared spectrogram; the infrared spectra were processed over a range of wavenumbers using OMNIC8.0Savitsky-Golay second derivative.
Preferably, the specification of the potassium bromide tablet is 8mm multiplied by 2mm to 3mm multiplied by 0.5mm, and more preferably 5mm multiplied by 1 mm;
preferably, the amount of the garlic seedling volatile oil for testing is 1-5 muL, and further preferably 2 muL;
preferably, the infrared spectrum has a scanning range of 6000cm-1～80cm-1More preferably 4000cm-1～400cm-1；
Preferably, the wave number range selected by the second derivative infrared of the processed infrared spectrogram is 4000cm-1～400cm-1Further preferably 2000cm-1～400cm-1；
Preferably, the specification of the potassium bromide tablet is 5mm multiplied by 1mm, and the garlic seedling volatile oilThe test amount of (2) is 2 mu L, and the scanning range of the infrared spectrum is 4000cm-1～400cm-1The wave number range of the second derivative infrared processing infrared spectrogram is 2000cm-1～400cm-1. Under the condition, the drawn infrared spectrogram can accurately identify the characteristic functional groups in the volatile oil of the garlic seedlings, and further proves qualitative and quantitative results obtained by gas chromatography-mass spectrometry; the second derivative infrared treatment can clearly show the structural difference of the volatile oil of the two garlic seedlings.
According to the third object of the invention, the invention provides the application of the garlic seedling volatile oil in the preparation of anticoagulant functional products; the volatile oil of garlic sprout comprises any one of volatile oil of garlic sprout or volatile oil of garlic yellow.
According to the fourth object of the invention, the invention provides an anticoagulant application of garlic seedling volatile oil, which is used for preparing a soft capsule preparation; the volatile oil of garlic sprout comprises any one of volatile oil of garlic sprout or volatile oil of garlic yellow; the soft capsule preparation comprises garlic seedling volatile oil, vegetable oil and capsule wall material;
preferably, the garlic seedling volatile oil is prepared from the following components in percentage by weight: the vegetable oil is 1:0 to 1:10, preferably 1:2 to 1: 5;
preferably, the vegetable oil is one of seabuckthorn oil, perilla oil, linseed oil, sunflower seed oil, corn oil, almond oil or olive oil; or the weight ratio of the sea buckthorn oil: 1-2: 3-5 of perilla oil, and sea buckthorn oil: 1-2: 3-5 parts of linseed oil, and 1-2: 3-5 parts of sea buckthorn oil: perilla oil: the linseed oil is a compound of two or more than two of 1-2: 2-5: 2-3.
The capsule wall material contains a sizing material, a plasticizer and water; preferably, the weight ratio of the rubber compound: a plasticizer is 1: 0.4-1: 0.6; water: the sizing material is 1: 0.5-1: 1.5;
preferably, the rubber compound is gelatin, gum arabic or a mixture of the two; the plasticizer is glycerol, sorbitol or a mixture of the glycerol and the sorbitol;
the preparation method of the soft capsule provided by the invention comprises a rotary die pressing method, a manual die pressing method and a dropping method; preferably, the rotary die pressing method is adopted, and the temperature is controlled to be 40-50 ℃.
The invention has the following beneficial effects:
the preparation method of the garlic seedling volatile oil provided by the invention fully exerts the mechanism synergistic advantages of microwave/ultrasound in the aspect of plant cell wall breaking, and the extraction time is obviously shorter than that of the traditional volatile oil extraction technology; the yield of the garlic sprout and the garlic yellow volatile oil prepared by the method is even higher than 0.22 +/-0.03-0.35 +/-0.01 percent of the reported garlic volatile oil (Food Chemistry,221, 196-204.).
Secondly, a gas chromatography-mass spectrometry combined technology (GC-MS) has certain errors in the qualitative and quantitative aspects of volatile oil, the infrared spectrum coupling second derivative infrared technology provided by the invention can assist in verifying the analysis result of the GC-MS, and can accurately identify the fine structure characteristics of similar natural products.
③ the garlic sprout and the volatile oil of the garlic clove exert the anticoagulation effect by activating the intrinsic, extrinsic and common blood coagulation ways and reducing the fibrinogen content; wherein, the garlic sprout volatile oil has better effect than the garlic clove volatile oil in activating intrinsic and extrinsic coagulation paths; the role of the volatile oil of the garlic clove yellow in activating the common blood coagulation path is superior to that of the volatile oil of the garlic sprout and is also superior to that of heparin; the garlic sprout and the volatile oil of the garlic yellow have the effect similar to that of the heparin in the aspect of reducing the content of the fibrinogen.
The garlic seedling volatile oil soft capsule provided by the invention can better cover the pungent smell of garlic seedlings and garlic yellow volatile oil, and the vegetable oil with the cardiovascular and cerebrovascular diseases preventing functions, such as sea buckthorn oil, perilla oil, linseed oil and the like, is selected as an oil-soluble matrix and can generate a synergistic effect with the garlic seedling volatile oil.
Drawings
FIG. 1 is a GC-MS total ion chromatogram of volatile oil of garlic sprouts;
FIG. 2 is a GC-MS total ion chromatogram of volatile oil of Garlic yellow.
FIG. 3 is an infrared spectrum of volatile oil of garlic sprout (EOGS) and volatile oil of blanched garlic leaf (EOBGS);
FIG. 4 is a second derivative infrared spectrum of volatile oil of garlic sprout (EOGS) and volatile oil of garlic clove (EOBGS);
Detailed Description
The volatile oil extraction device used in the examples was an 8-007-B volatile oil extractor available from Kenberg Bomei (Beijing) laboratory vessel Co., Ltd; the ultrasonic-microwave synergistic extractor is a DP-CW-2000 ultrasonic-microwave synergistic extractor which is purchased from Beijing Asia Oudepeng science and technology Limited.
EXAMPLE 1 preparation of volatile oil of garlic sprout and blanched garlic leaves
Weighing 100g of fresh garlic sprouts or garlic yellow, cutting into small sections of 1-2 cm, placing the small sections into a volatile oil extraction device, and soaking the small sections in distilled water at a ratio of 1:30 for 2 hours; placing the volatile oil extraction device in an ultrasonic-microwave synergistic extraction instrument, refluxing at 100-105 ℃, starting a microwave mode, adjusting to 600W, and extracting for 10 min; switching to an ultrasonic mode, adjusting to 70W, and extracting for 25 min; cooling, collecting volatile oil layer, further extracting and enriching water layer with dichloromethane as solvent, evaporating at 25-30 deg.C under reduced pressure to remove solvent, and mixing volatile oils to obtain volatile oils of garlic sprout and garlic yellow with extraction rates of 0.55 + -0.02% and 0.78 + -0.06%, respectively.
The extraction rate of the garlic sprout and the garlic clove yellow volatile oil is calculated according to the following method: the weight of the volatile oil is M (g), the fresh weight of the garlic sprouts and the garlic yellow is M (g), and M/M (w/w,%) is the extraction rate.
Comparative example
On the basis of example 1, in order to prove that the microwave/ultrasonic-assisted extraction method provided by the invention is superior to a single steam distillation method or a single microwave-assisted method or a single ultrasonic-assisted method, the invention designs the following comparative experiments:
scheme A: steam distillation method for preparing volatile oil of garlic sprout and garlic yellow
Weighing 100g of fresh garlic sprouts or garlic yellow, cutting into small sections of 1-2 cm, placing the small sections into a volatile oil extraction device, and soaking the small sections in distilled water at a ratio of 1:30 for 2 hours; extracting for 35min after refluxing at 100-105 ℃; cooling, collecting volatile oil layer, further extracting and enriching water layer with dichloromethane as solvent, vacuum evaporating at 25-30 deg.C to remove solvent, and mixing volatile oils to obtain garlic sprout and blanched garlic leaf volatile oil.
Extracting with water vapor for 35min without microwave or ultrasonic assisted extraction, wherein the extraction rates of volatile oil of garlic sprout and garlic clove are 0.04 + -0.002% and 0.06 + -0.001%, respectively.
Scheme B: microwave-assisted preparation of garlic sprout and garlic yellow volatile oil
Weighing 100g of fresh garlic sprouts and garlic yellow, cutting into small sections of 1-2 cm, placing the small sections into a volatile oil extraction device, and soaking the small sections in distilled water at a material-liquid ratio of 1:30 for 2 hours; placing the volatile oil extraction device in an ultrasonic-microwave synergistic extraction instrument, refluxing at 100-105 ℃, starting a microwave mode, adjusting to 600W, and extracting for 35 min; cooling, collecting volatile oil layer, further extracting and enriching water layer with dichloromethane as solvent, vacuum evaporating at 25-30 deg.C to remove solvent, and mixing volatile oils to obtain garlic sprout and blanched garlic leaf volatile oil.
Extracting under 600W microwave power for 35min to obtain volatile oil with extraction rates of 0.13 + -0.02% and 0.16 + -0.04% respectively.
Scheme C: ultrasonic-assisted preparation of garlic sprout and blanched garlic leaf volatile oil
Weighing 100g of fresh garlic sprouts and garlic yellow, cutting into small sections of 1-2 cm, placing the small sections into a volatile oil extraction device, and soaking the small sections in distilled water at a material-liquid ratio of 1:30 for 2 hours; placing the volatile oil extraction device in an ultrasonic-microwave synergistic extraction instrument, refluxing at 100-105 ℃, starting a microwave mode, adjusting to 70W, and extracting for 35 min; cooling, collecting volatile oil layer, further extracting and enriching water layer with dichloromethane as solvent, vacuum evaporating at 25-30 deg.C to remove solvent, and mixing volatile oils to obtain garlic sprout and blanched garlic leaf volatile oil.
Extracting under 70W ultrasonic power for 35min to obtain volatile oil with extraction rates of 0.18 + -0.05% and 0.21 + -0.03% respectively.
The comparative examples show that: within the same extraction time, the yield of the volatile oil extracted by single microwave or ultrasonic assistance is obviously higher than that of the steam distillation method; compared with example 1, the method is lower than the microwave/ultrasonic synergistic auxiliary extraction method. The reason for this is probably that although microwave and ultrasound can promote the wall breaking of plant cell walls and facilitate the release of active ingredients, the wall breaking mechanisms of the microwave and the ultrasound are different, the single use effect is not good in synergistic use effect, the synergistic use can generate the advantages of complementary wall breaking mechanisms and reduction of respective working time, and the release of the active ingredients is facilitated.
Example 2 gas chromatography-Mass Spectrometry analysis of volatile oil of garlic sprouts and blanched garlic leaves
The qualitative and quantitative analysis of the volatile oil of garlic sprout and garlic clove adopts Shimadzu GCMS-QP2010 gas chromatography-mass spectrometer. The analysis conditions were as follows: rxi-5Sil MS column (30 m.times.0.25 mm.times.0.25 μm); an ion trap detector; carrier gas: helium, flow rate: 1.0 mL/min; the temperatures of the transmission line and the detector are respectively set to be 250 ℃ and 230 ℃; the chromatographic column incubator adopts programmed temperature rise: setting the initial temperature at 40 deg.C, holding for 4min, raising to 60 deg.C at 5 deg.C/min, holding for 2min, raising to 110 deg.C at 15 deg.C/min, holding for 4min, raising to 180 deg.C at 5 deg.C/min, holding for 5min, raising to 280 deg.C at 25 deg.C/min, and holding for 5 min. Respectively dissolving the volatile oil of garlic sprout and garlic yellow in ether to prepare solution with the concentration of 12 mg/mL; injecting 1 mu L of the mixture into a chromatographic column, setting the split ratio to be 1:30, the ionization energy to be 70eV and the scanning range to be 35-500 amu. The components of the garlic sprout and the blanched garlic clove oil are identified by comparison with the National Institute of Standards and Technology (NIST) database and retention index.
FIG. 1 and FIG. 2 are GC-MS total ion current chromatograms of volatile oil of garlic sprout and garlic yellow. As can be seen from FIGS. 1 and 2, 31 kinds of volatile substances were detected from the volatile oil of garlic sprouts; 21 volatile substances were detected from the blanched garlic leaves volatile oil. As shown in table 1, 16 volatile compounds and 14 volatile compounds in the garlic sprout and the garlic clove yellow volatile oil were finally identified by exact matching with NIST database. Wherein the sulfur-containing compound is the main component and respectively accounts for 87.18% and 94.40% of the volatile oil of garlic sprout and garlic clove; diallyl disulfide is the most abundant compound (42.10% of volatile oil of garlic sprout and 45.13% of volatile oil of garlic clove); then diallyl trisulfide (accounting for 25.49% of the volatile oil of the garlic sprouts and 31.88% of the volatile oil of the garlic leaves) and diallyl tetrasulfide (accounting for 6.25% of the volatile oil of the garlic sprouts and 8.23% of the volatile oil of the garlic leaves) are added.
TABLE 1 chemical composition of volatile oil of garlic sprout and volatile oil of garlic clove.
Figure BDA0002449877110000081
Figure BDA0002449877110000091
RI is retention index.
EXAMPLE 3 Infrared Spectroscopy and Infrared second derivative Spectroscopy of volatile oil of Garlic sprout and Garlic yellow
In order to further prove qualitative and quantitative results obtained by gas chromatography-mass spectrometry combined analysis, the invention further adopts infrared spectroscopy to identify the garlic sprout and the garlic yellow volatile oil. Pressing the potassium bromide solid into a semitransparent sheet with the specification of 5mm multiplied by 1 mm; respectively and uniformly coating 2 mu L of garlic sprout and garlic yellow volatile oil on the slices; placing in an infrared spectrometer at 4000cm-1～400cm-1The scanning is performed in the wavenumber range.
As shown in FIG. 3, volatile oil from garlic sprout and garlic clove have similar infrared absorption peaks. Located at 3451.9cm-1The broad peak of (2) is attributed to the stretching vibration peak of the hydroxyl group in the alcohol compound; 3083.6cm-1、3012.3cm-1Respectively belong to vas(CH2CH-) and upsilonas(CH2＝CH-)；2925.5cm-1、2850.2cm-1、1421.3cm-1And 782.1cm-1Respectively belong to upsilonas(-CH2-)、υs(-CH2-)、δ(-CH2-) and gamma (-CH2-)；1847.5cm-1And 1716.3cm-1Attributing C to the stretching vibration of O; 1635.3cm-1Attributing C to C-C stretching vibration; 1459.8cm-1C-C belonging telescopic vibration; 1396.2cm-1And 1373.1cm-1Bending vibration of C-H in the home methyl; 1292.1cm-1C-H stretching vibration in the alkane; 1214.9cm-1And 1076.1cm-1C-O attributing telescopic vibration; 991.2cm-1And 917.9cm-1Respectively belong to omega (CH)2＝CH-) and ω (ωCH 2＝CH-)；858.2cm-1Home delta (CH)2＝CH-)；721.3cm-1Attributing C-S-C stretching vibration; 578.5cm-1And 472.5cm-1Respectively attributing to C-S and S-S stretching vibration. The infrared spectrum analysis result further proves that: garlic sprouts,The volatile oil of the garlic clove yellow contains alcohols, olefins, alkanes, esters and sulfur-containing compounds, which is consistent with the results of gas chromatography-mass spectrometry combined analysis shown in table 1.
In order to further search the difference of the garlic sprout and the volatile oil of the garlic yellow on the infrared spectrogram, the garlic sprout and the volatile oil of the garlic yellow are respectively treated by OMNIC8.0Savitsky-Golay second derivative at 2000cm-1～400cm-1Infrared spectrum in the wavenumber range.
As shown in fig. 4, at about 1032.5cm-1In the vicinity, a second derivative infrared spectrogram of the volatile oil of the blanched garlic leaves has a remarkable absorption peak, but the volatile oil of the garlic sprouts does not exist, the absorption peak is probably caused by stretching vibration of C-N in 1-methylpyrrolidine-2-thione, and the compound is only detected in the volatile oil of the blanched garlic leaves (Table 1). The second derivative infrared spectrogram can amplify fine structure difference, and is combined with the infrared spectrogram to be a powerful means for proving the characteristic functional groups of the garlic sprout and the garlic yellow volatile oil.
Example 4 evaluation of anticoagulant Effect of Garlic sprout and Garlic yellow volatile oil
Comprehensively evaluating the anticoagulant effect of the garlic sprout and the volatile oil of garlic yellow by four experiments of Prothrombin Time (PT), Thrombin Time (TT), activated partial prothrombin time (APTT) and Fibrinogen (FIB) content measurement; physiological saline is used as a negative control, and 30mg/mL heparin is used as a positive control; the experimental methods and procedures were referred to kit instructions.
As shown in Table 2, compared with normal saline, 3.75 mg/mL-30.0 mg/mL of volatile oil of garlic sprout and 15.0 mg/mL-30.0 mg/mL of volatile oil of blanched garlic bulb can obviously prolong the PT value (P is less than 0.01); when the concentration of the garlic sprout volatile oil is 30.0mg/mL, the PT value reaches 48.50 +/-3.06 s, which is obviously higher than that of the garlic yellow volatile oil (38.98 +/-1.91 s). This indicates that the garlic sprout volatile oil is superior to the garlic yellow volatile oil in activating extrinsic coagulation pathway.
Compared with normal saline, 3.75 mg/mL-30.0 mg/mL of garlic sprout volatile oil and 3.75 mg/mL-30.0 mg/mL of garlic clove volatile oil can obviously prolong the TT value (P is less than 0.01); when the concentration of the volatile oil of the blanched garlic leaves is 30.0mg/mL, the TT value reaches 216.9 +/-6.32 s, which is almost 3 times more than that of the volatile oil of the blanched garlic leaves (71.83 +/-1.65 s) and heparin (69.90 +/-3.12 s). This indicates that the volatile oil of garlic clove yellow is significantly superior to the volatile oil of garlic sprout and heparin in activating common coagulation pathway.
Compared with normal saline, 7.50 mg/mL-30.0 mg/mL of garlic sprout volatile oil and 15.0 mg/mL-30.0 mg/mL of garlic clove volatile oil can obviously prolong the APTT value (P is less than 0.01); when the concentration of the garlic sprout volatile oil is 30.0mg/mL, the APTT value reaches 87.77 +/-11.0 s, which is obviously higher than that of the garlic yellow volatile oil (49.63 +/-1.20 s). This indicates that the volatile oil of garlic sprout is superior to the volatile oil of garlic yellow in the aspect of endogenous blood coagulation.
Compared with normal saline, the 3.75 mg/mL-30.0 mg/mL garlic sprout volatile oil and 1.88 mg/mL-30.0 mg/mL garlic yellow volatile oil can obviously reduce the FIB content (P is less than 0.01); when the concentration of the volatile oil reaches 30.0mg/mL, the FIB content of the garlic sprout volatile oil group is 23.15 +/-1.98 mg/dL, the FIB content of the garlic yellow volatile oil group is 24.95 +/-2.85 mg/dL, the FIB content of the heparin group is 25.34 +/-3.39 mg/dL, and no statistical difference exists (P > 0.05). This shows that the volatile oil of garlic sprout and garlic yellow has the same effect of reducing FIB content as heparin.
In a word, the garlic sprout and the volatile oil of the garlic yellow play an anticoagulant role by activating intrinsic coagulation, extrinsic coagulation and common coagulation paths and reducing FIB content. Wherein, the role of the volatile oil of the garlic clove yellow in activating the intrinsic and extrinsic coagulation pathways is better than that of the volatile oil of the garlic clove yellow; the role of the volatile oil of the garlic clove yellow in activating the common blood coagulation path is superior to that of the volatile oil of the garlic sprout and is also superior to that of heparin; the effect of the garlic sprout and the volatile oil of the garlic yellow on the aspect of reducing the FIB content is close to that of the heparin.
TABLE 2 Effect of garlic sprout and garlic clove essential oil on PT, TT, APTT and FIB content.
Figure BDA0002449877110000121
Data are expressed as mean ± SD, averaging three experiments in the same column, different symbols in the superscript represent statistical differences (P <0.05 or, P <0.01).
EXAMPLE 5 preparation of Soft capsules of Garlic sprout and Garlic yellow volatile oil
A first soft capsule,
Putting 100g of gelatin and 100g of water into a glue pot for soaking; adding 50g of glycerol after the gelatin absorbs water and expands, heating to 70-80 ℃, and uniformly mixing; standing and preserving heat for 2h to enable the foam to float upwards, scraping the floating foam, filtering by white cloth, and preserving the heat of the filtrate for later use (A);
fully stirring 1g of garlic sprout volatile oil and 2g of seabuckthorn oil for later use (B);
loading the components (A) and (B) into an automatic rotary capsule rolling machine, and controlling the temperature at 40-50 ℃ to prepare the garlic sprout volatile oil soft capsule.
The volatile oil of garlic sprout in (B) is changed into volatile oil of garlic clove yellow, and the soft capsule of garlic clove yellow volatile oil can be prepared by the same method.
The second soft capsule,
Soaking 100g of Arabic gum and 100g of water in a gum pot; adding 50g of sorbitol after the Arabic gum absorbs water and expands, heating to 70-80 ℃, and uniformly mixing; standing and preserving heat for 2h to enable the foam to float upwards, scraping the floating foam, filtering by white cloth, and preserving the heat of the filtrate for later use (A);
fully stirring 1g of garlic sprout volatile oil and 2g of perilla herb oil for standby (B);
loading the components (A) and (B) into an automatic rotary capsule rolling machine, and controlling the temperature at 40-50 ℃ to prepare the garlic sprout volatile oil soft capsule.
The volatile oil of garlic sprout in (B) is changed into volatile oil of garlic clove yellow, and the soft capsule of garlic clove yellow volatile oil can be prepared by the same method.
Soft capsule III,
Putting 100g of gelatin and 100g of water into a glue pot for soaking; adding 50g of glycerol after the gelatin absorbs water and expands, heating to 70-80 ℃, and uniformly mixing; standing and preserving heat for 2h to enable the foam to float upwards, scraping the floating foam, filtering by white cloth, and preserving the heat of the filtrate for later use (A);
fully stirring 1g of garlic sprout volatile oil and 3g of linseed oil for later use (B);
loading the components (A) and (B) into an automatic rotary capsule rolling machine, and controlling the temperature at 40-50 ℃ to prepare the garlic sprout volatile oil soft capsule.
The volatile oil of garlic sprout in (B) is changed into volatile oil of garlic clove yellow, and the soft capsule of garlic clove yellow volatile oil can be prepared by the same method.
Four components of soft capsule,
Soaking 100g of Arabic gum and 100g of water in a gum pot; adding 50g of sorbitol after the Arabic gum absorbs water and expands, heating to 70-80 ℃, and uniformly mixing; standing and preserving heat for 2h to enable the foam to float upwards, scraping the floating foam, filtering by white cloth, and preserving the heat of the filtrate for later use (A);
fully stirring 1g of the garlic sprout volatile oil, 0.5g of sea buckthorn oil and 1.5g of perilla herb oil for standby (B);
loading the components (A) and (B) into an automatic rotary capsule rolling machine, and controlling the temperature at 40-50 ℃ to prepare the garlic sprout volatile oil soft capsule.
The volatile oil of garlic sprout in (B) is changed into volatile oil of garlic clove yellow, and the soft capsule of garlic clove yellow volatile oil can be prepared by the same method.
The soft capsule five,
Putting 100g of gelatin and 100g of water into a glue pot for soaking; adding 50g of glycerol after the gelatin absorbs water and expands, heating to 70-80 ℃, and uniformly mixing; standing and preserving heat for 2h to enable the foam to float upwards, scraping the floating foam, filtering by white cloth, and preserving the heat of the filtrate for later use (A);
fully stirring 1g of garlic sprout volatile oil, 0.7g of seabuckthorn oil and 2.1g of linseed oil for later use (B);
loading the components (A) and (B) into an automatic rotary capsule rolling machine, and controlling the temperature at 40-50 ℃ to prepare the garlic sprout volatile oil soft capsule.
The volatile oil of garlic sprout in (B) is changed into volatile oil of garlic clove yellow, and the soft capsule of garlic clove yellow volatile oil can be prepared by the same method.
Six soft capsules,
Putting 100g of gelatin and 100g of water into a glue pot for soaking; adding 50g of glycerol after the gelatin absorbs water and expands, heating to 70-80 ℃, and uniformly mixing; standing and preserving heat for 2h to enable the foam to float upwards, scraping the floating foam, filtering by white cloth, and preserving the heat of the filtrate for later use (A);
fully stirring 1g of the garlic sprout volatile oil, 0.5g of seabuckthorn oil, 1g of perilla oil and 1g of linseed oil for standby (B);
loading the components (A) and (B) into an automatic rotary capsule rolling machine, and controlling the temperature at 40-50 ℃ to prepare the garlic sprout volatile oil soft capsule.
The volatile oil of garlic sprout in (B) is changed into volatile oil of garlic clove yellow, and the soft capsule of garlic clove yellow volatile oil can be prepared by the same method.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (5)

1. A preparation method of garlic seedling volatile oil is characterized by comprising the following steps: weighing a certain amount of fresh garlic seedlings, cutting into small segments, placing in a volatile oil extraction device, and soaking with distilled water according to a certain material-liquid ratio;
placing the volatile oil extraction device in an ultrasonic-microwave synergistic extraction instrument, refluxing at 100-105 ℃, adjusting to a certain microwave power, and extracting for a certain time; switching to an ultrasonic mode, adjusting to a certain ultrasonic power, and extracting for a certain time;
cooling, collecting volatile oil layer, collecting water layer, further enriching volatile oil with dichloromethane as solvent, evaporating at low temperature under reduced pressure to remove solvent, and mixing oil layers to obtain volatile oil of garlic seedling;
the garlic seedlings comprise garlic sprouts and/or garlic yellow;
the volatile oil of garlic sprout comprises volatile oil of garlic sprout and/or volatile oil of garlic yellow; the main component in the garlic seedling volatile oil is a sulfur-containing compound, and the sulfur-containing compound comprises diallyl disulfide, diallyl trisulfide and diallyl tetrasulfide;
the feed liquid weight ratio of the fresh garlic sprouts and/or the garlic yellow to the distilled water is 1: 20-1: 50;
the microwave power is 400-800W; the microwave extraction time is 5-20 min;
the ultrasonic power is 50-100W; the ultrasonic extraction time is 10-40 min.
2. The method of claim 1, wherein: the feed liquid weight ratio of the fresh garlic seedlings to the distilled water is 1: 30; the microwave power is 600W, and the microwave extraction time is 10 min; the ultrasonic power is 70W, and the ultrasonic extraction time is 25 min.
3. A method for identifying garlic seedling volatile oil by infrared spectrum coupling second derivative infrared technology is characterized by comprising the following steps: the garlic seedling volatile oil is prepared by the method of claim 1, and the analysis result of gas chromatography-mass spectrometry is further proved by adopting an infrared spectrum coupling second derivative infrared technology;
the specific method comprises the following steps: loading the dried potassium bromide solid powder into a tablet machine, and pressing into potassium bromide tablets with certain specifications; uniformly coating a certain amount of garlic seedling volatile oil on the surface of a potassium bromide tablet; placing in an infrared spectrometer, scanning within a certain wave number range, and drawing an infrared spectrogram; processing an infrared spectrogram in a certain wave number range by using an OMNIC8.0Savitsky-Golay second derivative;
the specification of the potassium bromide tablet is 8mm multiplied by 2 mm-3 mm multiplied by 0.5 mm; the amount of the garlic seedling volatile oil for testing is 1-5 muL; the infrared spectrum has a scanning range of 6000cm-1 ~ 80 cm-1(ii) a The wave number range of the second derivative infrared selection for processing the infrared spectrogram is 4000cm−1 ~ 400 cm−1。
4. The method of claim 3, wherein: the specification of the potassium bromide tablet is 5mm multiplied by 1 mm; the amount of the garlic seedling volatile oil for testing is 2 muL; the infrared spectrum has a scanning range of 4000cm−1 ~ 400 cm−1(ii) a The wave number range of the second derivative infrared selection for processing the infrared spectrogram is 2000cm−1 ~ 400 cm−1。
5. The application of the garlic seedling volatile oil is characterized in that: the garlic seedling volatile oil prepared by the method of claim 1 is used for preparing an anticoagulant soft capsule, and the soft capsule comprises the garlic seedling volatile oil, vegetable oil and a capsule wall material;
according to the weight ratio, the garlic seedling volatile oil: vegetable oil = 1: 0-1: 10;
the vegetable oil is any one of seabuckthorn oil, perilla oil, linseed oil, sunflower seed oil, corn oil, almond oil or olive oil;
the capsule wall material contains a sizing material, a plasticizer and water; according to the weight ratio, the rubber material is as follows: plasticizer = 1: 0.4-1: 0.6; water: sizing material = 1: 0.5-1: 1.5; the sizing material is gelatin, Arabic gum or a mixture of the gelatin and the Arabic gum; the plasticizer is glycerin, sorbitol or a mixture of the glycerin and the sorbitol.
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