CN102924969A - Method for refining paprika red pigment - Google Patents

Abstract

The invention discloses a method for refining paprika red pigment. The method comprises the following steps of: dissolving capsicum oleoresin with distilled water; mixing ethanol with ammonia water to prepare a hot remover; adding twice quantities of hot remover into the capsicum oleoresin for stirring and separating to obtain the paprika red pigment; and adding 1-3 times of the quantity of the distilled water into the paprika red pigment to uniformly mix and deodorize for 2-3h under a vacuum condition to finish a refining process. By the method, each index of the paprika red pigment is effectively improved; a color value reaches 200-250; the capsaicine content is less than or equal to 0.005 percent; the acetone-insoluble substance content is less than or equal to 0.2 percent; and the solvent residues are less than 25 mg/kg without obvious characteristic smell. The used edulcoration agent, the hot remover and the deodorant are toxicity-free and harmless solvents, so that the method is simple in required equipment during the whole refining process, low in cost, simple in process and easy to operate, and lays a foundation for large-scale industrial production; and the exhaustion of waste gas and the drainage of waste water are substantially avoided.

Description

A kind of method of refining chilli haematochrome

Technical field

The invention belongs to the natural organic chemistry field, specifically relate to a kind of method of refining chilli haematochrome.

Background technology

Natural plant pigment is widely used in the industries closely bound up with HUMAN HEALTH such as food-processing, medicine and makeup as tinting material.Along with the development of biotechnology, the research and development of natural plant pigment are subject to people's attention day by day, and application prospect is very extensive.

Capsanthin is that a kind of security is good and the natural food colour of certain nutritive value and pharmacological action is arranged, and is just classified as one of four kinds of natural pigments giving priority to by country as far back as the enforcement period of the seventh five-year plan.In recent years, rise along with people's back to nature, pursuit health and green consumption trend, the chemosynthesis pigment that those once had been widely used, although its lovely luster, strong coloring force, stable in properties, cheap, but because it exists without nutritive value, chemical toxicity is arranged, can produce objectionable impurities and also may be by weakness such as heavy metal contamination such as As or Pb in building-up process simultaneously in the body metabolism process, their usage quantitys at home and abroad constantly reduce, and this just provides more wide market for natural pigments such as capsanthins.

Capsanthin is refining mainly contain take off peppery, take off the operation such as residual, deodorization, most critical be take off peppery.At present removing spiciness from capsicum red pigment mainly utilizes concentration to be 76%(v/v) ethanol fully mix with oleoresin capsicum as taking off peppery solvent, make capsaicine be dissolved in ethanol mutually in, utilize the haematochrome phase to carry out centrifugation with ethanol difference in specific gravity mutually, ethanol phase concentration and recovery ethanol, haematochrome phase precipitation obtains capsanthin.The method to take off peppery efficient on the low side, haematochrome takes off to need the peppery solvent of taking off of triplication to take off continuously without pungent peppery more than three times; Secondly, in process of production, alcohol concn is difficult to guarantee that concentration is high, and the pigment loss is large, and concentration is low, and light phase, heavy phase are difficult to separate.

The peppery method of taking off that also has is to take off peppery solvent with 70～100% methyl alcohol conduct, and the material ratio that takes off peppery solvent and oleoresin capsicum is 2:1, take off continuously peppery 2～3 times after, can reach requirement, but the toxicity of methyl alcohol is large, the injury to human body is larger in process of production.

Adopt chromatographic column to separate and take off in the peppery method, Chinese patent CN1392201A utilizes macroporous adsorbent resin to separate, and it is large to exist solvent-oil ratio, complicated operation, and yield is low, and large-scale industrial production is difficult to form.Present industrial use is more, and to be that organic solvent takes off peppery, and such as Chinese patent CN1035621C, CN1082570A etc., but exist the pigment recovery rate low take off the problems such as peppery number of times is too much, cause production efficiency not high.

Another refining problem of capsanthin is deodorization.Small-scale production adopts supercritical CO ₂The extraction deodorization, its advantage is that deodorization is thorough, such as Chinese patent CN1267684A, can remove preferably peculiar smell after adding the entrainment agent several times, but limit industrializing implementation with supercritical fluid technology; The problems such as Chinese patent CN1272385C is deodorizing composition with the mixed solvent of dehydrated alcohol and Virahol, also can remove preferably peculiar smell, but exists solvent consumption large, and deodorization time is long.

Summary of the invention

The object of the invention is to for the deficiencies in the prior art, the process for purification of the capsanthin that a kind of technique is simple, production cost is low, product yield is high is provided.

Purpose of the present invention is achieved by the following technical programs.

Except as otherwise noted, percentage ratio of the present invention is mass percent.

A kind of method of refining chilli haematochrome, the method may further comprise the steps:

(1) under 25 ℃～80 ℃ conditions, oleoresin capsicum and the water material ratio (g/mL) by 1:1～10:1 is mixed, stir 1 h～4 h;

(2) step with centrifugal separation (1) gained mixed solution, remove water-soluble impurity after, obtain the refining chilli oleo-resinous;

(3) with 60%(v/v) ethanol and ammoniacal liquor is in 2:1～5:1(v/v) ratio is mixed with spicy-off agency; Add 2 times of amount spicy-off agencies in the refining chilli oleo-resinous, then under 20 ℃～50 ℃ conditions, stir 0.5 h～2.0 h, leave standstill centrifugation mixed solution behind 20 min～30 min, once taken off peppery oleoresin capsicum; Repeat again describedly to take off peppery program once with once taking off the peppery oleoresin capsicum that obtains, take off oleoresin capsicum after peppery and reclaim solvent and obtain capsanthin;

(4) add the distilled water of 1～3 times of amount in the capsanthin that step (3) obtains, after mixing, under the vacuum tightness of 0.05 Mpa～0.09 Mpa, 40 ℃～60 ℃ temperature condition, deodorization 2 h～3 h namely obtain the refining chilli haematochrome.

Relatively and prior art, the present invention has following beneficial effect:

Effective Raise the indices of product, the look valency of capsanthin reaches 200～250, capsaicine≤0.005%, acetone insoluble matter≤0.2%, dissolvent residual≤25 mg/kg is without the obvious characteristic smell;

2. the cleaner, spicy-off agency, the deodorizing composition that adopt all are nontoxic solvents, and whole treating process required equipment is simple, and cost is low, and essentially no waste gas, discharge of wastewater have no adverse effect to environment.

3. the simple easy handling of technique is for large-scale industrial production lays the first stone.

Embodiment

In order to make purpose of the present invention, technical scheme and advantage clearer, below in conjunction with embodiment the present invention is described in further detail.Should be appreciated that specific embodiment described herein only is used for explaining the present invention, be not intended to limit the present invention.

Embodiment 1

(the look valency is 151.3 with 1120 g oleoresin capsicums, acetone insoluble matter 3.1%, dissolvent residual 2236.8 mg/kg, capsaicine 0.08%) be added in the beaker of 3000 mL, then add the distilled water of 300 mL, 55 ℃ of heating in water bath stir 2 h, separate the refining chilli oleo-resinous 956.3 g(look valencys 171.4 that obtain, acetone insoluble matter 0.6%, dissolvent residual 1327.5 mg/kg, capsaicine 0.08%).Refining chilli oleo-resinous obtained above is added in the beaker of 5000 mL, add 1910 g spicy-off agencies (60% ethanol and ammoniacal liquor ratio are 4:1), at 35 ℃ of lower 1 h that stir, separate rapidly after leaving standstill 30 min, and then repeat to take off once peppery, reclaim solvent, obtain capsanthin 605.4 g(look valencys 249.4).The capsanthin that obtains is added in the matrass of 2000 mL, the distilled water that adds 630 g, control vacuum tightness 0.05 Mpa～0.09 Mpa deodorization, 2 h in 50 ℃ of water-baths, obtain at last high-quality capsanthin (the look valency 247.1 of 595.7 g, acetone insoluble matter 0.17%, dissolvent residual 16.7 mg/kg, capsaicine 0.0043%).

Capsanthin look valency of the present invention, dissolvent residual, capsaicine are measured according to GB GB10783-2008, and acetone insoluble matter is measured according to SN/T 0802.2-1999.

Capsanthin yield: 86.86%

The total look valency of 1120 g oleoresin capsicums: 1120 * 151.3=169456

Take off the peppery refining rear total look valency of capsanthin: 595.7 * 247.1=147197.5

Capsanthin yield: 147197.5/16945=86.86%.

Embodiment 2

(the look valency is 156.4 with 1270 g oleoresin capsicums, acetone insoluble matter 3.7%, dissolvent residual 2576.1 mg/kg, capsaicine 0.08%) is added in the beaker of 2000 mL, then adds the distilled water of 410 mL, heated and stirred 2 h between 70 ℃ of water-baths, separate the refining chilli oleo-resinous 1100 g(look valencys 173.5 that obtain, acetone insoluble matter 0.5%, dissolvent residual 1091.4 mg/kg, capsaicine 0.08%).Refining chilli oleo-resinous obtained above is added in the beaker of 5000 mL, add 2200 g spicy-off agencies (60% ethanol and ammoniacal liquor ratio are 5:1), at 40 ℃ of lower 1 h that stir, separate rapidly after leaving standstill 30 min, and then repeat to take off once peppery, reclaim solvent, obtain capsanthin 748.3 g(look valencys 230.1).Capsanthin obtained above is added in the matrass of 3000 mL, the distilled water that adds 1200 mL, control vacuum tightness 0.05 Mpa～0.09 Mpa deodorization, 3 h in 55 ℃ water-bath, obtain at last high-quality capsanthin (the look valency 228.3 of 736.3 g, acetone insoluble matter 0.58%, dissolvent residual 18.9 mg/kg, capsaicine 0.0019%).

Capsanthin yield: 84.63%

The total look valency of 1270 g oleoresin capsicums: 1270 * 156.4=198628

Take off the peppery refining rear total look valency of capsanthin: 736.3 * 228.3=168097.3

Capsanthin yield: 168097.3/198628=84.63%.

Comparative example (traditional process for purification)

(the look valency is 153.9, acetone insoluble matter 2.8%, dissolvent residual 2152.4 mg/kg with 1070 g oleoresin capsicums, capsaicine 0.08%) is added in the beaker of 5000ml, then add 2000ml 76%(v/v) ethanol, stir 0.5 h under the room temperature, leave standstill rapidly centrifugation behind 30 min, and then repeat to take off once peppery, reclaim solvent, obtain refining rear capsanthin 736.3g(look valency 176.5, acetone insoluble matter 0.91%, dissolvent residual 17.3 mg/kg, capsaicine 0.0096%).

Capsanthin yield: 78.92%

The total look valency of 1120 g oleoresin capsicums: 1070 * 153.9=164673

Take off the peppery refining rear total look valency of capsanthin: 736.3 * 176.5=129956.95

Capsanthin yield: 129956.95/164673=78.92%.

The contrast situation

For the present invention relatively makes with extra care the difference that ethanol the most frequently used in the production method takes off capsicum with the traditional technology capsanthin, the below is contrasted the product indices that inventive embodiments and comparative example obtain, and specifically sees the following form.

Table 1

	Embodiment 1	Embodiment 2	The ratio example
				The total look valency of raw material	169465	198628	164673
Total look valency after refining	147204.88	168095.04	129956.95
				Yield (%)	86.86	84.63	78.92
The look valency	247.1	228.3	186.5
				Acetone insoluble matter (%)	0.17	0.58	0.91
Dissolvent residual (mg/kg)	16.7	18.9	17.3
				Peppery degree (%)	0.0043	0.0019	0.0096
Smell	++	+	++++

Annotate: the light and heavy degree of "+" expression smell, smell is heavier, and "+" is more.

As can be seen from the above table, the every data of the present invention are compared with former traditional technology, and yield obviously improves, and other every quality index are also occupied certain advantage.

Claims (1)

1. the method for a refining chilli haematochrome, the method may further comprise the steps:

(1) under 25 ℃～80 ℃ conditions, oleoresin capsicum and the water material ratio by 1:1～10:1 is mixed, stir 1 h～4 h;

(2) step with centrifugal separation (1) gained mixed solution, remove water-soluble impurity after, obtain the refining chilli oleo-resinous;

(3) 60% ethanol and ammoniacal liquor are mixed with spicy-off agency in 2:1～5:1 ratio; Add 2 times of amount spicy-off agencies in the refining chilli oleo-resinous, then under 20 ℃～50 ℃ conditions, stir 0.5 h～2.0 h, leave standstill centrifugation mixed solution behind 20 min～30 min, once taken off peppery oleoresin capsicum; Repeat again describedly to take off peppery program once with once taking off the peppery oleoresin capsicum that obtains, take off oleoresin capsicum after peppery and reclaim solvent and obtain capsanthin;

(4) add the distilled water of 1～3 times of amount in the capsanthin that step (3) obtains, after mixing, under the vacuum tightness of 0.05 Mpa～0.09 Mpa, 40 ℃～60 ℃ temperature condition, deodorization 2 h～3 h namely obtain the refining chilli haematochrome.