CN105670784A - Method for extracting and purifying jujube kernel volatile oil - Google Patents
Method for extracting and purifying jujube kernel volatile oil Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
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- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
- A23D9/02—Other edible oils or fats, e.g. shortenings, cooking oils characterised by the production or working-up
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- C11B1/10—Production of fats or fatty oils from raw materials by extracting
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- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/108—Production of fats or fatty oils from raw materials by extracting after-treatment, e.g. of miscellae
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Abstract
The invention discloses a method for extracting and purifying jujube kernel volatile oil. The method comprises the following steps: (1) pretreatment of jujube kernel raw materials; (2) charging; (3) setting the temperature and pressure of an extraction kettle, a separation kettle I and a separation kettle II; (4) performing static extraction; (5) performing dynamic primary extraction; (6) performing dynamic secondary extraction; (7) merging the jujube kernel volatile oil obtained in the separation kettle I and the separation kettle II; and (8) performing column chromatography separation and purification of the jujube kernel volatile oil obtained in the step (7). In the invention, by adopting an extraction way combining static extraction and dynamic extraction, the extraction efficiency of jujube kernel volatile oil is greatly improved; and meanwhile, by selecting a proper extraction agent, the content of anti-oxidant compounds in the volatile oil is remarkably increased.
Description
Technical field
The invention belongs to technical field of natural plant active ingredient extraction, be specifically related to extraction and the purification process of a kind of Semen Ziziphi Spinosae volatile oil.
Background technology
Semen Ziziphi Spinosae (ZizyphusjujubeMill) is the kernel of Rhamnaceae jujube Fructus Jujubae class drying and ripening, and Semen Ziziphi Spinosae mainly contains the compounds such as Semen Ziziphi Spinosae saponins, triterpenes, fatty oil, protein, sterols, phospholipid. Modern pharmacological research shows: Semen Ziziphi Spinosae has reinforcing the heart, calmness, calms the nerves, arresting sweating, tonifying liver, the effect such as promote the production of body fluid, for restlessness of asrhenia type and insomnia, frightened dreaminess, body void hyperhidrosis, Tianjin wound waits disease yearningly, is the sedative hypnotics class comparatively commonly used. Beginning to be loaded in Shennong's Herbal, be classified as top grade, Compendium of Material Medica is classified as this category. See " Treatise on Febrile and Miscellaneous Disease " at the beginning of doctor's nationality, and famous with Semen Ziziphi Spinosae soup, the medicinal history of existing more than 1700 year. It was loaded in modern age and went through an edition Pharmacopoeia of the People's Republic of China. Volatile oil is one of Semen Ziziphi Spinosae main active, and in recent years, Semen Ziziphi Spinosae oil shows have the sedative-hypnotic effect identical with Semen Ziziphi Spinosae Fructus Gleditsia constituents after deliberation, has been an important research content of Semen Ziziphi Spinosae gradually.
The extraction of current Semen Ziziphi Spinosae volatile oil and the substantially following several method of purification process: steam distillation, organic solvent extraction and supercritical fluid extraction. All there is the problems such as yield is low, technique is loaded down with trivial details, operating condition is unstable in first two method, and supercritical CO2Fluids extraction is extraction and separation technology emerging at present, it is especially suitable for extracting heat-sensitive substance, and both heavy metal free pollutions, no solvent residue, and conveniently transport, the advantages such as extraction conditions is stable, and in extraction process, add appropriate entrainer, it is possible to it is effectively improved the yield of target product, but still exists and extract the problem that oil yield is relatively low.
Current Xinjiang jujube cultivation area has reached 7,000,000 mu, and the abundant developmental research that Fructus Jujubae resource is Semen Ziziphi Spinosae provides advantageous advantage, and Fructus Jujubae processing had become the important step of Xinjiang woods fruit plant husbandry scale and increasing peasant income already.
Summary of the invention
Present invention aims to Semen Ziziphi Spinosae and extract the low problem that cannot effectively utilize with raw material of oil yield, it is proposed to a kind of employing supercritical CO2Fluids extraction extracts and the method for volatile oil in purification Semen Ziziphi Spinosae.
The extraction of a kind of Semen Ziziphi Spinosae volatile oil and purification process, comprise the steps:
(1) pretreatment of Semen Ziziphi Spinosae raw material: Semen Ziziphi Spinosae is dried, pulverizes and sieves, standby;
(2) charging: the Semen Ziziphi Spinosae raw material of pretreatment is added supercritical CO2In the extraction kettle of fluid extraction device;
(3) extraction kettle, separating still I and the temperature of separating still II, pressure are set;
(4) static extracting: pass into a certain amount of CO2Make to rise in extraction kettle predetermined pressure, first carry out static extracting with solvent orange 2 A for entrainer;
(5) dynamic single extraction: regulation and control CO2Flow velocity, then carry out dynamic single extraction with solvent orange 2 A for entrainer;
(6) dynamic reextraction: regulation and control CO2Flow velocity, be eventually adding solvent B and carry out dynamic reextraction as entrainer;
(7) separating still I and separating still II obtain Semen Ziziphi Spinosae volatile oil merge;
(8) the Semen Ziziphi Spinosae volatile oil obtained in column chromatographic isolation and purification step (7), removes mobile phase and obtains Semen Ziziphi Spinosae volatile oil sterling.
The extraction of above-mentioned Semen Ziziphi Spinosae volatile oil and purification process, in step (1): Semen Ziziphi Spinosae is dried temperature and is 45-65 DEG C, and drying time is 15-25h, and the powder size after pulverizing and sieving is 50-70 order.
The extraction of above-mentioned Semen Ziziphi Spinosae volatile oil and purification process, in step (3): the extracting pressure of extraction kettle is 20-35MPa, and extraction temperature is 35-50 DEG C, the static extracting time is 0.5-1h, the dynamic single extraction time is 1-2h, and the dynamic reextraction time is 2-3h; The separating pressure of separating still I is 8.0-9.0MPa, and separation temperature is 30-40 DEG C, and disengaging time is 1-3h; The separating pressure of separating still II is 4.9-5.8MPa, and separation temperature is 30-40 DEG C, and disengaging time is 0.5-2h.
The extraction of above-mentioned Semen Ziziphi Spinosae volatile oil and purification process, in step (4) and (5): solvent orange 2 A is the one of normal hexane, ethyl acetate and chloroform.
The extraction of above-mentioned Semen Ziziphi Spinosae volatile oil and purification process, in step (6): solvent B is the mixture of n-butyl alcohol, t-butyl methyl ether or n-butyl alcohol and t-butyl methyl ether.
The extraction of above-mentioned Semen Ziziphi Spinosae volatile oil and purification process, in step (5) and (6): the flow of CO2 is 1.0-1.5L/min.
The extraction of above-mentioned Semen Ziziphi Spinosae volatile oil and purification process, the consumption of solvent orange 2 A is the 20-30wt% of Semen Ziziphi Spinosae raw materials quality, and the consumption of solvent B is the 50-100wt% of Semen Ziziphi Spinosae raw materials quality.
The extraction of above-mentioned Semen Ziziphi Spinosae volatile oil and purification process, in step (8): a) chromatographic column: ACQUITYUPLCBEHC18 post, 2.1mm × 50mm, 1.7 μm; B) mobile phase is by A phase and B phase composition: A phase is: methanol, and B phase is: 1mmol/L ammonium formate aqueous solution; C) condition of gradient elution: time initial, A phase and B phase volume ratio are 10:1, when 1 minute, A phase and B phase volume ratio are 8:3, when 3 minutes, A phase and B phase volume ratio are 7:4, when 6 minutes, A phase and B phase volume ratio are 6:5, and when 9 minutes, A phase and B phase volume ratio are 5:6, and when 12 minutes, A phase and B phase volume ratio are 4:7, when 15 minutes, A phase and B phase volume ratio are 3:8, when 18 minutes, A phase and B phase volume ratio are 1:10, start acquisition time: 1min, terminate acquisition time: 18min; D) column temperature: 35 DEG C; E) flow velocity: 0.6mL/ minute.
The extraction of above-mentioned Semen Ziziphi Spinosae volatile oil and purification process, also include in step (1) being sequentially carried out the Semen Ziziphi Spinosae raw material after pulverizing and sieving that alkali soaks, acid soak is gentle rushes solution soaking and dry step; The aqueous slkali that alkali immersion uses is mass concentration is the sodium carbonate liquor of 5-12wt%, and the aqueous slkali consumption of every 100g Semen Ziziphi Spinosae powder is 300-400mL, and alkali soak time is 5-10h, and alkali filters after soaking; The acid solution that acid soak uses is mass concentration is the hydrochloric acid of 10-15wt%, and the aqueous slkali consumption of every 100g Semen Ziziphi Spinosae powder is 200-300mL, and the acid soak time is 0.5-2h, filters after acid soak;Buffer solution soaks the phosphate buffer solution that the buffer solution used is pH=7.2, and buffer solution soak time is 5-10h.
The invention has the beneficial effects as follows: with Xinjiang, large woods arnotto Fructus Jujubae by-product Semen Ziziphi Spinosae is raw material to the present invention, supercritical carbon dioxide fluid extraction is utilized to extract the volatile oil in Semen Ziziphi Spinosae, by the extraction mode adopting static extracting and dynamic reextraction to combine, substantially increase the extraction efficiency of Semen Ziziphi Spinosae volatile oil, simultaneously by selecting suitable extractant and column chromatography purification technology to substantially increase the content of anti-oxidant compound in volatile oil, increase medical value and the practical value of Semen Ziziphi Spinosae volatile oil, improve the utilization rate of Semen Ziziphi Spinosae, add its economic benefit.
Detailed description of the invention
Embodiment 1:
The extraction of a kind of Semen Ziziphi Spinosae volatile oil and purification process, comprise the steps:
(1) pretreatment of Semen Ziziphi Spinosae raw material: be 45 DEG C in temperature and Semen Ziziphi Spinosae is dried 15h, pulverize and sieve, powder size is 50-70 order, standby;
(2) charging: the Semen Ziziphi Spinosae raw material of pretreatment is added supercritical CO together with solvent orange 2 A2In the extraction kettle of fluid extraction device; In the present embodiment, solvent orange 2 A is normal hexane; The consumption of solvent orange 2 A is the 20wt% of Semen Ziziphi Spinosae raw materials quality;
(3) extraction kettle, separating still I and the temperature of separating still II, pressure are set;
The extracting pressure of extraction kettle is 20MPa, and extraction temperature is 35 DEG C; The separating pressure of separating still I is 8.0MPa, and separation temperature is 30 DEG C; The separating pressure of separating still II is 4.9MPa, and separation temperature is 30 DEG C;
(4) static extracting: pass into a certain amount of CO2Making to rise to the setting pressure in step (3) in extraction kettle, first carry out static extracting with solvent orange 2 A for entrainer, the static extracting time is 0.5h;
(5) dynamic single extraction: regulation and control CO2Flow be 1.0L/min, then carry out dynamic single extraction with solvent orange 2 A for entrainer, the dynamic single extraction time is 1h;
(6) dynamic reextraction: regulation and control CO2Flow be 1.0L/min, finally carry out dynamic reextraction as entrainer with entrainer pump to extraction kettle adds solvent B, the dynamic reextraction time is 2h; Solvent B is n-butyl alcohol, and the consumption of solvent B is the 50wt% of Semen Ziziphi Spinosae raw materials quality;
(7) in separating still I, disengaging time is 1h, and in separating still II, disengaging time is 0.5h, separating still I and separating still II obtains Semen Ziziphi Spinosae volatile oil and merges;
(8) the Semen Ziziphi Spinosae volatile oil obtained in column chromatographic isolation and purification step (7), a) chromatographic column: ACQUITYUPLCBEHC18 post, 2.1mm × 50mm, 1.7 μm; B) mobile phase is by A phase and B phase composition: A phase is: methanol, and B phase is: 1mmol/L ammonium formate aqueous solution; C) condition of gradient elution: time initial, A phase and B phase volume ratio are 10:1, when 1 minute, A phase and B phase volume ratio are 8:3, when 3 minutes, A phase and B phase volume ratio are 7:4, when 6 minutes, A phase and B phase volume ratio are 6:5, and when 9 minutes, A phase and B phase volume ratio are 5:6, and when 12 minutes, A phase and B phase volume ratio are 4:7, when 15 minutes, A phase and B phase volume ratio are 3:8, when 18 minutes, A phase and B phase volume ratio are 1:10, start acquisition time: 1min, terminate acquisition time: 18min; D) column temperature: 35 DEG C; E) flow velocity: 0.6mL/ minute; Remove mobile phase and obtain Semen Ziziphi Spinosae volatile oil sterling.
Through weighing the quality finally giving Semen Ziziphi Spinosae volatile oil, the productivity obtaining Semen Ziziphi Spinosae volatile oil is 21.15%, and the total antioxidant capacity adopting T-AOC RNA isolation kit test volatile oil is 18.17 units/mg.
Embodiment 2:
The extraction of a kind of Semen Ziziphi Spinosae volatile oil and purification process, comprise the steps:
(1) pretreatment of Semen Ziziphi Spinosae raw material: be 65 DEG C in temperature and Semen Ziziphi Spinosae is dried 25h, pulverize and sieve, powder size is 50-70 order, standby;
(2) charging: the Semen Ziziphi Spinosae raw material of pretreatment is added supercritical CO together with solvent orange 2 A2In the extraction kettle of fluid extraction device; In the present embodiment, solvent orange 2 A is ethyl acetate; The consumption of solvent orange 2 A is the 30wt% of Semen Ziziphi Spinosae raw materials quality;
(3) extraction kettle, separating still I and the temperature of separating still II, pressure are set;
The extracting pressure of extraction kettle is 35MPa, and extraction temperature is 50 DEG C; The separating pressure of separating still I is 9.0MPa, and separation temperature is 40 DEG C; The separating pressure of separating still II is 5.8MPa, and separation temperature is 40 DEG C;
(4) static extracting: pass into a certain amount of CO2Making to rise to the setting pressure in step (3) in extraction kettle, first carry out static extracting with solvent orange 2 A for entrainer, the static extracting time is 1h;
(5) dynamic single extraction: regulation and control CO2Flow be 1.5L/min, then carry out dynamic single extraction with solvent orange 2 A for entrainer, the dynamic single extraction time is 2h;
(6) dynamic reextraction: regulation and control CO2Flow be 1.5L/min, finally carry out dynamic reextraction as entrainer with entrainer pump to extraction kettle adds solvent B, the dynamic reextraction time is 3h; Solvent B is t-butyl methyl ether, and the consumption of solvent B is the 100wt% of Semen Ziziphi Spinosae raw materials quality;
(7) in separating still I, disengaging time is 3h, and in separating still II, disengaging time is 2h, separating still I and separating still II obtains Semen Ziziphi Spinosae volatile oil and merges;
(8) the Semen Ziziphi Spinosae volatile oil obtained in column chromatographic isolation and purification step (7), a) chromatographic column: ACQUITYUPLCBEHC18 post, 2.1mm × 50mm, 1.7 μm; B) mobile phase is by A phase and B phase composition: A phase is: methanol, and B phase is: 1mmol/L ammonium formate aqueous solution; C) condition of gradient elution: time initial, A phase and B phase volume ratio are 10:1, when 1 minute, A phase and B phase volume ratio are 8:3, when 3 minutes, A phase and B phase volume ratio are 7:4, when 6 minutes, A phase and B phase volume ratio are 6:5, and when 9 minutes, A phase and B phase volume ratio are 5:6, and when 12 minutes, A phase and B phase volume ratio are 4:7, when 15 minutes, A phase and B phase volume ratio are 3:8, when 18 minutes, A phase and B phase volume ratio are 1:10, start acquisition time: 1min, terminate acquisition time: 18min; D) column temperature: 35 DEG C; E) flow velocity: 0.6mL/ minute; Remove mobile phase and obtain Semen Ziziphi Spinosae volatile oil sterling.
Through weighing the quality finally giving Semen Ziziphi Spinosae volatile oil, the productivity obtaining Semen Ziziphi Spinosae volatile oil is 23.11%, and the total antioxidant capacity adopting T-AOC RNA isolation kit test volatile oil is 19.88 units/mg.
Embodiment 3:
The extraction of a kind of Semen Ziziphi Spinosae volatile oil and purification process, comprise the steps:
(1) pretreatment of Semen Ziziphi Spinosae raw material: be 50 DEG C in temperature and Semen Ziziphi Spinosae is dried 17h, pulverize and sieve, powder size is 50-70 order, standby;
(2) charging: the Semen Ziziphi Spinosae raw material of pretreatment is added supercritical CO together with solvent orange 2 A2In the extraction kettle of fluid extraction device; In the present embodiment, solvent orange 2 A is the one of chloroform; The consumption of solvent orange 2 A is the 22wt% of Semen Ziziphi Spinosae raw materials quality;
(3) extraction kettle, separating still I and the temperature of separating still II, pressure are set;
The extracting pressure of extraction kettle is 30MPa, and extraction temperature is 40 DEG C; The separating pressure of separating still I is 8.5MPa, and separation temperature is 35 DEG C; The separating pressure of separating still II is 5.0MPa, and separation temperature is 35 DEG C;
(4) static extracting: pass into a certain amount of CO2Making to rise to the setting pressure in step (3) in extraction kettle, first carry out static extracting with solvent orange 2 A for entrainer, the static extracting time is 0.8h;
(5) dynamic single extraction: regulation and control CO2Flow be 1.2L/min, then carry out dynamic single extraction with solvent orange 2 A for entrainer, the dynamic single extraction time is 1.5h;
(6) dynamic reextraction: regulation and control CO2Flow be 1.3L/min, finally carry out dynamic reextraction as entrainer with entrainer pump to extraction kettle adds solvent B, the dynamic reextraction time is 2.5h; Solvent B is the mixture of n-butyl alcohol and t-butyl methyl ether, and the consumption of solvent B is the 60wt% of Semen Ziziphi Spinosae raw materials quality;
(7) in separating still I, disengaging time is 2h, and in separating still II, disengaging time is 1h, separating still I and separating still II obtains Semen Ziziphi Spinosae volatile oil and merges;
(8) the Semen Ziziphi Spinosae volatile oil obtained in column chromatographic isolation and purification step (7), a) chromatographic column: ACQUITYUPLCBEHC18 post, 2.1mm × 50mm, 1.7 μm; B) mobile phase is by A phase and B phase composition: A phase is: methanol, and B phase is: 1mmol/L ammonium formate aqueous solution; C) condition of gradient elution: time initial, A phase and B phase volume ratio are 10:1, when 1 minute, A phase and B phase volume ratio are 8:3, when 3 minutes, A phase and B phase volume ratio are 7:4, when 6 minutes, A phase and B phase volume ratio are 6:5, and when 9 minutes, A phase and B phase volume ratio are 5:6, and when 12 minutes, A phase and B phase volume ratio are 4:7, when 15 minutes, A phase and B phase volume ratio are 3:8, when 18 minutes, A phase and B phase volume ratio are 1:10, start acquisition time: 1min, terminate acquisition time: 18min; D) column temperature: 35 DEG C; E) flow velocity: 0.6mL/ minute; Remove mobile phase and obtain Semen Ziziphi Spinosae volatile oil sterling.
Through weighing the quality finally giving Semen Ziziphi Spinosae volatile oil, the productivity obtaining Semen Ziziphi Spinosae volatile oil is 22.75%, and the total antioxidant capacity adopting T-AOC RNA isolation kit test volatile oil is 20.45 units/mg.
Embodiment 4:
The extraction of a kind of Semen Ziziphi Spinosae volatile oil and purification process, comprise the steps:
(1) pretreatment of Semen Ziziphi Spinosae raw material: be 60 DEG C in temperature and Semen Ziziphi Spinosae is dried 23h, pulverize and sieve, powder size is 50-70 order, standby;
(2) charging: the Semen Ziziphi Spinosae raw material of pretreatment is added supercritical CO together with solvent orange 2 A2In the extraction kettle of fluid extraction device; In the present embodiment, solvent orange 2 A is ethyl acetate; The consumption of solvent orange 2 A is the 25wt% of Semen Ziziphi Spinosae raw materials quality;
(3) extraction kettle, separating still I and the temperature of separating still II, pressure are set;
The extracting pressure of extraction kettle is 32MPa, and extraction temperature is 45 DEG C; The separating pressure of separating still I is 8.3MPa, and separation temperature is 33 DEG C; The separating pressure of separating still II is 5.4MPa, and separation temperature is 36 DEG C;
(4) static extracting: pass into a certain amount of CO2Making to rise to the setting pressure in step (3) in extraction kettle, first carry out static extracting with solvent orange 2 A for entrainer, the static extracting time is 0.7h;
(5) dynamic single extraction: regulation and control CO2Flow be 1.4L/min, then carry out dynamic single extraction with solvent orange 2 A for entrainer, the dynamic single extraction time is 1.5h;
(6) dynamic reextraction: regulation and control CO2Flow be 1.4L/min, finally carry out dynamic reextraction as entrainer with entrainer pump to extraction kettle adds solvent B, the dynamic reextraction time is 2.2h; Solvent B is the volume ratio of the mixture of n-butyl alcohol and t-butyl methyl ether, n-butyl alcohol and t-butyl methyl ether is 1:3, and the consumption of solvent B is the 80wt% of Semen Ziziphi Spinosae raw materials quality;
(7) in separating still I, disengaging time is 2.5h, and in separating still II, disengaging time is 1.5h, separating still I and separating still II obtains Semen Ziziphi Spinosae volatile oil and merges;
(8) the Semen Ziziphi Spinosae volatile oil obtained in column chromatographic isolation and purification step (7), a) chromatographic column: ACQUITYUPLCBEHC18 post, 2.1mm × 50mm, 1.7 μm;B) mobile phase is by A phase and B phase composition: A phase is: methanol, and B phase is: 1mmol/L ammonium formate aqueous solution; C) condition of gradient elution: time initial, A phase and B phase volume ratio are 10:1, when 1 minute, A phase and B phase volume ratio are 8:3, when 3 minutes, A phase and B phase volume ratio are 7:4, when 6 minutes, A phase and B phase volume ratio are 6:5, and when 9 minutes, A phase and B phase volume ratio are 5:6, and when 12 minutes, A phase and B phase volume ratio are 4:7, when 15 minutes, A phase and B phase volume ratio are 3:8, when 18 minutes, A phase and B phase volume ratio are 1:10, start acquisition time: 1min, terminate acquisition time: 18min; D) column temperature: 35 DEG C; E) flow velocity: 0.6mL/ minute; Remove mobile phase and obtain Semen Ziziphi Spinosae volatile oil sterling.
Through weighing the quality finally giving Semen Ziziphi Spinosae volatile oil, the productivity obtaining Semen Ziziphi Spinosae volatile oil is 23.26%, and the total antioxidant capacity adopting T-AOC RNA isolation kit test volatile oil is 20.19 units/mg.
Embodiment 5:
The present embodiment and embodiment 1 are distinctive in that: also include in step (1) being sequentially carried out the Semen Ziziphi Spinosae raw material after pulverizing and sieving that alkali soaks, acid soak is gentle rushes solution soaking and dry step; The aqueous slkali that alkali immersion uses is mass concentration is the sodium carbonate liquor of 5wt%, and the aqueous slkali consumption of every 100g Semen Ziziphi Spinosae powder is 300mL, and alkali soak time is 5h, and alkali filters after soaking; The acid solution that acid soak uses is mass concentration is the hydrochloric acid of 10wt%, and the aqueous slkali consumption of every 100g Semen Ziziphi Spinosae powder is 200mL, and the acid soak time is 0.5h, filters after acid soak; Buffer solution soaks the phosphate buffer solution that the buffer solution used is pH=7.2, and buffer solution soak time is 5h.
Through weighing the quality finally giving Semen Ziziphi Spinosae volatile oil, the productivity obtaining Semen Ziziphi Spinosae volatile oil is 23.82%, and the total antioxidant capacity adopting T-AOC RNA isolation kit test volatile oil is 22.63 units/mg.
Embodiment 6:
The present embodiment and embodiment 2 are distinctive in that: also include in step (1) being sequentially carried out the Semen Ziziphi Spinosae raw material after pulverizing and sieving that alkali soaks, acid soak is gentle rushes solution soaking and dry step; The aqueous slkali that alkali immersion uses is mass concentration is the sodium carbonate liquor of 12wt%, and the aqueous slkali consumption of every 100g Semen Ziziphi Spinosae powder is 400mL, and alkali soak time is 10h, and alkali filters after soaking; The acid solution that acid soak uses is mass concentration is the hydrochloric acid of 15wt%, and the aqueous slkali consumption of every 100g Semen Ziziphi Spinosae powder is 300mL, and the acid soak time is 2h, filters after acid soak; Buffer solution soaks the phosphate buffer solution that the buffer solution used is pH=7.2, and buffer solution soak time is 10h.
Through weighing the quality finally giving Semen Ziziphi Spinosae volatile oil, the productivity obtaining Semen Ziziphi Spinosae volatile oil is 24.31%, and the total antioxidant capacity adopting T-AOC RNA isolation kit test volatile oil is 23.27 units/mg.
Embodiment 7:
The present embodiment and embodiment 3 are distinctive in that: also include in step (1) being sequentially carried out the Semen Ziziphi Spinosae raw material after pulverizing and sieving that alkali soaks, acid soak is gentle rushes solution soaking and dry step; The aqueous slkali that alkali immersion uses is mass concentration is the sodium carbonate liquor of 10wt%, and the aqueous slkali consumption of every 100g Semen Ziziphi Spinosae powder is 350mL, and alkali soak time is 8h, and alkali filters after soaking; The acid solution that acid soak uses is mass concentration is the hydrochloric acid of 12wt%, and the aqueous slkali consumption of every 100g Semen Ziziphi Spinosae powder is 250mL, and the acid soak time is 1h, filters after acid soak; Buffer solution soaks the phosphate buffer solution that the buffer solution used is pH=7.2, and buffer solution soak time is 8h.
Through weighing the quality finally giving Semen Ziziphi Spinosae volatile oil, the productivity obtaining Semen Ziziphi Spinosae volatile oil is 23.71%, and the total antioxidant capacity adopting T-AOC RNA isolation kit test volatile oil is 21.01 units/mg.
Embodiment 8:
The present embodiment and embodiment 4 are distinctive in that: also include in step (1) being sequentially carried out the Semen Ziziphi Spinosae raw material after pulverizing and sieving that alkali soaks, acid soak is gentle rushes solution soaking and dry step; The aqueous slkali that alkali immersion uses is mass concentration is the sodium carbonate liquor of 7wt%, and the aqueous slkali consumption of every 100g Semen Ziziphi Spinosae powder is 360mL, and alkali soak time is 9h, and alkali filters after soaking; The acid solution that acid soak uses is mass concentration is the hydrochloric acid of 11wt%, and the aqueous slkali consumption of every 100g Semen Ziziphi Spinosae powder is 300mL, and the acid soak time is 2h, filters after acid soak; Buffer solution soaks the phosphate buffer solution that the buffer solution used is pH=7.2, and buffer solution soak time is 6h.
Through weighing the quality finally giving Semen Ziziphi Spinosae volatile oil, the productivity obtaining Semen Ziziphi Spinosae volatile oil is 30.05%, and the total antioxidant capacity adopting T-AOC RNA isolation kit test volatile oil is 25.37 units/mg.
By embodiment 5-8 it can be seen that after being sequentially carried out that alkali soaks, acid soak is gentle and rushing solution soaking, the productivity of Semen Ziziphi Spinosae volatile oil can be greatly improved, and the total antioxidant capacity change of gained volatile oil is little. But, if alkali soaks, acid soak is eased up, and the order rushing solution soaking changes, reduce by more than 26% when the productivity of Semen Ziziphi Spinosae volatile oil not only can be made relatively not soak, and also can reduce by more than 8% when the total antioxidant capacity of volatile oil is not soaked relatively.
Above-described embodiment is only for clearly demonstrating the invention example, and is not the restriction to the invention detailed description of the invention. For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description. Here without also cannot all of embodiment be given exhaustive. All any apparent changes extended out within the spirit and principles in the present invention or variation are still among the invention scope of the claims.
Claims (9)
1. the extraction of a Semen Ziziphi Spinosae volatile oil and purification process, it is characterised in that comprise the steps:
(1) pretreatment of Semen Ziziphi Spinosae raw material: Semen Ziziphi Spinosae is dried, pulverizes and sieves, standby;
(2) charging: the Semen Ziziphi Spinosae raw material of pretreatment is added supercritical CO2In the extraction kettle of fluid extraction device;
(3) extraction kettle, separating still I and the temperature of separating still II, pressure are set;
(4) static extracting: pass into a certain amount of CO2Make to rise in extraction kettle predetermined pressure, first carry out static extracting with solvent orange 2 A for entrainer;
(5) dynamic single extraction: regulation and control CO2Flow velocity, then carry out dynamic single extraction with solvent orange 2 A for entrainer;
(6) dynamic reextraction: regulation and control CO2Flow velocity, be eventually adding solvent B and carry out dynamic reextraction as entrainer;
(7) separating still I and separating still II obtain Semen Ziziphi Spinosae volatile oil merge;
(8) the Semen Ziziphi Spinosae volatile oil obtained in column chromatographic isolation and purification step (7), removes mobile phase and obtains Semen Ziziphi Spinosae volatile oil sterling.
2. the extraction of Semen Ziziphi Spinosae volatile oil according to claim 1 and purification process, it is characterised in that
In step (1): Semen Ziziphi Spinosae is dried temperature and is 45-65 DEG C, and drying time is 15-25h, and the powder size after pulverizing and sieving is 50-70 order.
3. the extraction of Semen Ziziphi Spinosae volatile oil according to claim 1 and purification process, it is characterised in that
In step (3): the extracting pressure of extraction kettle is 20-35MPa, and extraction temperature is 35-50 DEG C, the static extracting time is 0.5-1h, and the dynamic single extraction time is 1-2h, and the dynamic reextraction time is 2-3h;The separating pressure of separating still I is 8.0-9.0MPa, and separation temperature is 30-40 DEG C, and disengaging time is 1-3h; The separating pressure of separating still II is 4.9-5.8MPa, and separation temperature is 30-40 DEG C, and disengaging time is 0.5-2h.
4. the extraction of Semen Ziziphi Spinosae volatile oil according to claim 1 and purification process, it is characterised in that
In step (4) and (5): solvent orange 2 A is the one of normal hexane, ethyl acetate and chloroform.
5. the extraction of Semen Ziziphi Spinosae volatile oil according to claim 1 and purification process, it is characterised in that
In step (6): solvent B is the mixture of n-butyl alcohol, t-butyl methyl ether or n-butyl alcohol and t-butyl methyl ether.
6. the extraction of Semen Ziziphi Spinosae volatile oil according to claim 1 and purification process, it is characterised in that
In step (5) and (6): CO2Flow be 1.0-1.5L/min.
7. the extraction of Semen Ziziphi Spinosae volatile oil according to claim 4 and purification process, it is characterised in that
The consumption of solvent orange 2 A is the 20-30wt% of Semen Ziziphi Spinosae raw materials quality, and the consumption of solvent B is the 50-100wt% of Semen Ziziphi Spinosae raw materials quality.
8. the extraction of Semen Ziziphi Spinosae volatile oil according to claim 1 and purification process, it is characterised in that in step (8): a) chromatographic column: ACQUITYUPLCBEHC18 post, 2.1mm × 50mm, 1.7 μm; B) mobile phase is by A phase and B phase composition: A phase is: methanol, and B phase is: 1mmol/L ammonium formate aqueous solution; C) condition of gradient elution: time initial, A phase and B phase volume ratio are 10:1, when 1 minute, A phase and B phase volume ratio are 8:3, when 3 minutes, A phase and B phase volume ratio are 7:4, when 6 minutes, A phase and B phase volume ratio are 6:5, and when 9 minutes, A phase and B phase volume ratio are 5:6, and when 12 minutes, A phase and B phase volume ratio are 4:7, when 15 minutes, A phase and B phase volume ratio are 3:8, when 18 minutes, A phase and B phase volume ratio are 1:10, start acquisition time: 1min, terminate acquisition time: 18min; D) column temperature: 35 DEG C; E) flow velocity: 0.6mL/ minute.
9. according to the extraction of the arbitrary described Semen Ziziphi Spinosae volatile oil of claim 1-8 and purification process, it is characterized in that, in step (1), also include being sequentially carried out the Semen Ziziphi Spinosae raw material after pulverizing and sieving that alkali soaks, acid soak is gentle rushes solution soaking and dry step; The aqueous slkali that alkali immersion uses is mass concentration is the sodium carbonate liquor of 5-12wt%, and the aqueous slkali consumption of every 100g Semen Ziziphi Spinosae powder is 300-400mL, and alkali soak time is 5-10h, and alkali filters after soaking; The acid solution that acid soak uses is mass concentration is the hydrochloric acid of 10-15wt%, and the aqueous slkali consumption of every 100g Semen Ziziphi Spinosae powder is 200-300mL, and the acid soak time is 0.5-2h, filters after acid soak; Buffer solution soaks the phosphate buffer solution that the buffer solution used is pH=7.2, and buffer solution soak time is 5-10h.
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