CN106512018B - A kind of refined honey method suitable for honeyed bolus - Google Patents
A kind of refined honey method suitable for honeyed bolus Download PDFInfo
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Abstract
The present invention discloses a kind of sweet method of the white silk suitable for big honeyed bolus.A kind of refined honey method suitable for the production of big honeyed bolus, step are as follows: (1) select honey for raw material；(2) raw material honey is pumped into jacketed pan, opens jacketed pan steam valve, interlayer is passed through steam under constant stirring, and honey is warming up to 75-85 DEG C, refines 5-15h, is continuously heating to 105-120 DEG C, boils 0.5-2h, places 5-15h after steam off valve；(3) honey after standing is then sent to cold boiler through the screen to filtrate；(4) in cold boiler, under condition of negative pressure, concentration refining is carried out, observes photoelectricity refractometer, controls moisture；(5) honey refined is inputted into storage honey jar.The present invention practices honey using method of the jacketed pan steam heating normal pressure in conjunction with vacuum-concentrcted, and stability is good, and the loss of preparation process effective component is low, quality is high, easy to operate.
Description
Technical field
Practice sweet method suitable for big honeyed bolus the present invention relates to a kind of.
Background technique
Honeyed bolus is a kind of most widely used dosage form of tcm clinical practice, is played a very important role in Chinese materia medica preparation.Honey
Ball property is stablized, and carrying is easy to use, and toxic side effect is small, as the excipient or corrigent in preparation, can mitigate pharmacological property, increases
The effect of curative effect of drug, reinforcement drug tonifying middle-Jiao and Qi, moistening lung to arrest cough.
Rich in the nutriments such as sugar abundant, organic acid, vitamin in honey, under there is nourishing to relieving asthma, delay, defaecation, solution
The effects of malicious.Modern study explanation, the honey after processing can enhance the solubility of aglycon in certain medicinal materials in order to absorb, and
Have reproducibility and anti-corrosive antibacterial effect, it can be to avoid the oxidation deterioration of effective component in medicinal material, it is ensured that the quality of drug.But
It is that honey contains 25% or so moisture, a portion is moisture inferior, separately there is the impurity such as dead bee, wax, starchy material.
Wax can float on pill surface, form very thin wax coat, and depositing can crack long, and then finished product is dry and cracked when starch-containing class is more.
Therefore, honey has to pass through refining before entering ball, to remove impurity, destroys ferment, kills microorganism, suitably reduction moisture, increases
Add bonding force.
According to refining temperature and finished product feature, refined honey is divided into tender honey, middle sweet and old honey, wherein tender honey heating temperature is
105-115 DEG C, 20% or more water content, five significant change of color, slightly stickiness；Middle honey heating temperature is 116-119 DEG C, aqueous
10%-13% is measured, color has stickiness in faint yellow；The old hot temperature of honey is 119-122 DEG C, and water content is lower than 4%, and color is in reddish brown
Color has strong tack, that is, is easy to be heated the limitation of method and condition.Thus while having so specific data regulation, in reality
It is not widely used in the work of border.
Honey refining quality directly affects the quality of sweet scorching drug and honeyed bolus.If refining is inadequate, honeyed bolus is in storage period
Easily there are elephant skin, mouldy, stiff, rupture, sand return and other issues, therefore, needs to carry out quality in refining process stringent
Monitoring.Traditional refining fado is refined using normal pressure, i.e., boiling water (or adding boiling boiling in honey) is added in honey, makes to dissolve,
And suitably dilute, by three to No. four sieves to filter out impurity, filtrate is set in copper pot and is heated, and constantly skimming, stirring, until needing
Degree.Modern refined honey mainly uses refining temperature as Con trolling index, but still needs to according to prescription traditional Chinese medicine powder water content and Drug
Matter grasps refining degree.
Currently, generalling use jacketed pan steam heating normal pressure refined honey.But due to the ununified technological principle of refined honey and have
The quality requirement of pass causes various regions enterprise to carry out refined honey using different temperature and times, causes the quality of refined honey irregular,
It is easy to appear the excessively soft or really up to the mark phenomenon of finished product, influences beauty, or even causes the honeyed bolus moisture absorption, mildew or hard, or even influences medicine
Product curative effect.According to data, there are no the specific honey of clear stipulaties to refine work for Chinese Pharmacopoeia and each province and city medicinal material processing specification
The quality standard of skill and refined honey, therefore, researching and developing one kind has the governed honeyed bolus refined honey method of quality standard, is urgently to be resolved at present
Problem.
Summary of the invention
Of the invention is to influence quality to solve finished product of the existing technology refining and be easy to appear really up to the mark or excessively soft
The problem of with curative effect, and provide a kind of stability is good, preparation process effective component lose low, quality it is high be suitable for it is big
The refined honey method of honeyed bolus production.
The present invention is achieved by the following technical solutions:
A kind of refined honey method suitable for the production of big honeyed bolus,
(1) raw material selects: selecting honey for raw material；
(2) normal pressure is refined: raw material honey being pumped into jacketed pan, jacketed pan steam valve is opened, presss from both sides under constant stirring
Layer is passed through steam, and honey is warming up to 75-85 DEG C, refines 5-15h, is continuously heating to 105-120 DEG C, boils 0.5-2h, closes and steams
Steam valve places 5-15h behind the door；
(3) the screen to filtrate: by the honey after standing through the screen to filtrate, it is then sent to cold boiler；
(4) negative pressure is refined: in cold boiler, under condition of negative pressure, concentration refining is carried out, observes photoelectricity refractometer,
Control moisture；
(5) honey refined is inputted into storage honey jar.
Further, sticky syrupy shape creamy white or light yellow is selected or thick if congealed fat shape semifluid honey is raw material.
When the normal pressure is refined, it is passed through 0.1-0.5Mpa steam under agitation.
When the negative pressure is refined, vacuum degree 0.04-0.08Mpa.
It is described to carry out concentration refining under condition of negative pressure, it is that moisture is controlled by observation photoelectricity refractometer.
The present invention utilizes jacketed pan, using refined honey method of the heating normal pressure in conjunction with vacuum-concentrcted, overcomes existing
The problem of finished product existing for technology is really up to the mark or excessively soft, influences quality and curative effect.Specifically, first, the present invention use normal pressure
The refined honey method combined with vacuum concentration method, non-pressure process control refined honey quality, and vacuum-concentrcted method controls moisture content；Its
Secondary, honey has good antioxidant activity after processing, the reason is that in honey carbohydrate content (69-86%) based on monosaccharide, wherein
Fructose content accounts for about 38%, and glucose content accounts for about 31%, and high-temperature heating can make sugar that caramelization, sugared caramelization occur
Product has preferable antioxidant activity, and 5-HMF, phenols etc. also have good inoxidizability, and refined honey of the present invention is first in the process
It is warming up to 75-85 DEG C of refining, this step generates 5-HMF by glucose more cyclodehydrations that are heated；Temperature rises to 105- after 5-15h
120 DEG C of tanning 0.5-2h, fructose participate in reaction, and the polyphenol content of generation increases significant, inoxidizability enhancing, DPPH clearance rate ratio
Big more when first step fructose, glucose coexist, therefore, the 5-HMF generated during refined honey is relatively fewer, and inoxidizability is shown
It writes；Again, the extension of heating time, the raising of heating temperature, color burn and the antioxidation enhancing of honey, the face of honey
It is significant related between color and antioxidant activity, but the refined honey time was lost more than the nutriment in time honey of the present invention
In serious, refined honey loses the meaning originally having；Finally, existing honey refining process disunity, criteria of quality evaluation lack, cause to refine
Honey quality be difficult to control, the present invention on the basis of existing technology, by polyphenol content measurement, 5-HMF content, measurement of pH etc.
As the index ingredient of quality control, and 5-HMF assay keeps result more accurate using high-efficient liquid phase technique, preferably controls
Refined honey quality, phenolic substances are the important activity ingredients of honey, and phenolic hydroxyl structure especially ortho position phenolic hydroxyl group is easily oxidized
At quinones structure, with the very strong ability for removing free radical.Polyphenol can be big with protein (enzyme), polysaccharide, alkaloid and biology
Molecule recombination reaction, in addition the activity of its own removing free radical having, makes it have more physiological activity, it is such as anti-to lure
Change, anti-aging etc..Polyphenol content is the strong and weak important measurement standard of honey activity, it may be possible to influence honey refining front and back pharmacological property and change
The key of change, 5-HMF are not present in fresh honey, and with being continuously increased in processing or ageing process.5-HMF is influenced to contain
, such as temperature and the heating time, pH, Hua Yuan a lot of because being known as of amount, therefore 5-HMF content can be used as the detection excessively heated
Index.
In refining process of the present invention, stringent quality control is carried out to refined honey:
(1) sample preparation: when refining in aforementioned manners, taking sample 50g at interval of 25 DEG C, each temperature spot take wherein 2g arrive
Test tube, distilled water dissolve and are settled to 25ml, and 4000rpm is centrifuged 20 minutes, takes supernatant, obtain the honey sample of 80mg/ml, use
In analysis physicochemical property.
(2) total phenol content measures: measuring total phenol content using Folin-Ciocalteu method, prepares solution and reference substance
Solution, wherein the preparation method of the sodium carbonate liquor of 1mol/L is that precision weighs 21.2g natrium carbonicum calcinatum, and distilled water dissolution is fixed
Hold 200mL, shake up to obtain the final product；The preparation of gallic acid reference substance solution is that precision weighs 10mg gallic acid reference substance, with steaming
Simultaneously constant volume shakes up to 10mL up to 1.0mg/mL gallic acid reference substance stock solution for distilled water dissolution；Take stock solution appropriate, it is dilute with water
It is interpreted into the series standard solution that concentration is 5,10,25,50,80,100 μ g/mL；
Specific assay method is as follows: taking 100 μ L honey samples (80mg/mL) or gallic acid standard solution, adds l00 μ L
Folin-Ciocalteu color developing agent, after mixing, add the sodium carbonate liquor of 0.5mL mol/L, 300 μ L of distilled water, room temperature,
1h is placed under the conditions of being protected from light, and measures absorbance under 760nm.
(3) 5-HMF assay:
The preparation of reference substance solution: first dissolving 0.011g 5-HMF standard items, and constant volume to 10mL is configured to 1.1mg/mL
Stoste, then it is diluted with water to the series standard solution of 0.011,0.022,0.11,0.22,1.1,11,22 μ g/mL；
The pretreatment of sample: taking honey sample, is diluted with water 8 times, and with 0.45 μm of filtering with microporous membrane, gained filtrate is used
HPLC is detected；
Chromatographic condition: chromatographic column: C18Chromatographic column (150mm × 4.6mm, 5 μm)；Mobile phase: acetonitrile: 0.1% phosphoric acid solution=
4:92；Column temperature: 25 DEG C；Detection wavelength: wavelength 284nm；Flow velocity: 1mL/min；Sample volume: 20 μ L；It is accurate respectively to draw standard items
Solution and each 20 μ L of sample solution, inject liquid chromatograph, measurement to get.
(4) it colour measurement: is measured by absorbance of the 80mg/ml honey sample at 420nm.
(5) pH value measures: being counted and is measured by PH.
In order to verify effect of the present invention, quality determination is carried out to according to finished product made from this method for the present invention
1, total phenol content measures
(1) drafting of gallic acid standard curve
The measurement of total phenol content is to use gallic acid as standard in honey, is measured using Folin-Ciocalteu method,
With gallic acid concentration C (μ g/mL) for abscissa, the absorbance value A at 760nm is ordinate mapping, as shown in Figure 1, gained
Data are as shown in table 1, and linear recurrence handles to obtain calibration curve equation: A=0.23926x-0.21207, R2=0.99011,
It is linear between 5 μ g/mL to 100 μ g/mL.
1 gallic acid standard curve of table
(2) sample total phenol content measurement result
TPC is calculated according to gallic acid standard curve in honey refining process, and content range is arrived in 90.84 μ g/g
Between 1236.28 μ g/g, 14 times are increased, as shown in Fig. 2, the results are shown in Table 2, figure it is seen that with refined honey temperature
Raising, total phenol content constantly increases, and elevation amplitude is gradually steady at 125 DEG C or so.
Total phenol content changes in 2 honey refining process of table
2,5-HMF assay result
(1) specificity is analyzed: under measurement chromatographic condition, 5-HMF peak shape is good, divides in sample liquid with other chromatographic peaks
It is good from degree, as a result as shown in Figure 3,4.
(2) lower limit of quantitation measurement result
The measurement result of lower limit of quantitation is shown in Table 3, S/N > 10, calculating RSD value is 0.95% (n=6), bat
It is 100.19%, illustrates that lower limit of quantitation meets sample measurement and requires.
3 lower limit of quantitation of table (0.1100 μ g/mL) investigates result data (n=6)
(3) linear relationship is investigated
The measurement of 5-HMF reference substance solution standard curve is as shown in figure 5, the results are shown in Table 4, standard curve regression equation
Are as follows: A=145.1C-2.7313, R2=0.99992,5-HMF concentration within the scope of 0.0110 ~ 22 μ g/mL, linear relationship is good.
4 5-HMF standard curve of table
(4) precision measurement result
According to the degree of closeness of the measurement concentration of 5-HMF reference substance solution and theoretical actual concentration, the precision of method is investigated
Degree.Measurement result see the table below.
5 precision data result of table
Precision RSD value is 1.43% (n=6), bat 98.73%, the results showed that this method precision conforms to
It asks.
(5) repeated measurement result
It is 0.40% that the measurement result of repeated experiment, which is shown in Table 6, RSD value,.Illustrate that this method repeatability result meets inspection and wants
It asks.
6 method repeatability data result (n=5) of table
(6) Stability Determination result
Stability Determination the results are shown in Table 7, with the measurement concentration calculation RSD value of 5-HMF content in sample for 0.2%, illustrate quilt
Sample is stablized in 24 hours.
7 stability test data result of table
| Time (h) | 0 | 1 | 2 | 4 | 8 | 12 | 24 | Mean value | RSD% |
| Measured value (mg/mL) | 4.6872 | 4.6904 | 4.6893 | 4.7125 | 4.7073 | 4.7005 | 4.6997 | 4.6981 | 0.20 |
(7) sample-adding recycling measurement result
The measurement result of sample-adding recovery experiment is shown in Table 8, and average recovery rate 99.3620%, RSD value is 0.76%, illustrates this
Measuring method is reliable.
Table 8 is loaded recovery experiment test data result (n=5)
3, colour measurement result
Color change measurement result is shown in Table 9 in honey refining process,
Color change (80mg/mL) in 9 honey refining process of table
The result shows that honey after processing is handled color intensity have significant change.
4, acid-base property measurement result
The pH value of the refining honey measured under different temperatures is as shown in table 10,
PH value variation (80mg/mL) in 10 honey refining process of table
| Processing temperature/DEG C | 0 | 25 | 50 | 75 | 100 | 125 | 150 |
| PH value | 3.95 | 4.02 | 4.10 | 4.15 | 3.98 | 3.80 | 3.77 |
As shown in table 10, the range that pH value changes in honey refining process is between 3.77 to 4.15, at the initial stage of processing
PH value rises to 4.15 from 3.95 in 75min, drops to 3.77 again during 75min to 150min.There is early stage in honey sample
The reason of pH rises may be caused by original certain acidic materials are decomposed by thermal response in honey, and the reduction of later period pH value is then
It may be as caused by the generation degradation such as nonenzymatic browning reaction and fructose.
Compared with prior art, the present invention is practiced using method of the jacketed pan steam heating normal pressure in conjunction with vacuum-concentrcted
Honey, stability is good, and the loss of preparation process effective component is low, quality is high, easy to operate.
Detailed description of the invention
Fig. 1 is gallic acid canonical plotting；
Fig. 2 is total phenol content variation in refining process；
Fig. 3 is reference substance 5-HMF figure；
Fig. 4 is 100 minutes honey 5-HMF figures of refining；
Fig. 5 is 5-HMF canonical plotting.
Specific embodiment
The invention will be further described with reference to embodiments.
Embodiment 1
A kind of refined honey method suitable for the production of big honeyed bolus,
(1) raw material selects: selecting the sticky syrupy shape honey of milky is raw material；
(2) normal pressure is refined: raw material honey being pumped into jacketed pan, jacketed pan steam valve is opened, presss from both sides under constant stirring
Layer is passed through 0.4-0.5Mpa steam, and honey is warming up to 75-85 DEG C, refines 5h, is continuously heating to 105-120 DEG C, boils 1h, closes
12h is placed after steam valve；
(3) the screen to filtrate: by the honey after standing through the screen to filtrate, it is then sent to cold boiler；
(4) negative pressure is refined: in cold boiler, in the case where vacuum degree is 0.04-0.05Mpa condition of negative pressure, being concentrated
Refining controls moisture；
(5) honey refined is inputted into storage honey jar.
Embodiment 2
A kind of refined honey method suitable for the production of big honeyed bolus,
(1) raw material selects: selecting thick if congealed fat shape semifluid honey is raw material；
(2) normal pressure is refined: raw material honey being pumped into jacketed pan, jacketed pan steam valve is opened, presss from both sides under constant stirring
Layer is passed through 0.3-0.4Mpa steam, and honey is warming up to 75-85 DEG C, refines 8h, is continuously heating to 105-120 DEG C, boils 0.5h, closes
8h is placed after closing steam valve；
(3) the screen to filtrate: by the honey after standing through the screen to filtrate, it is then sent to cold boiler；
(4) negative pressure is refined: in cold boiler, in the case where vacuum degree is 0.05-0.06Mpa condition of negative pressure, being concentrated
Photoelectricity refractometer is observed in refining, controls moisture；
(5) honey refined is inputted into storage honey jar.
Embodiment 3
A kind of refined honey method suitable for the production of big honeyed bolus,
(1) raw material selects: selecting the sticky syrupy shape honey of milky is raw material；
(2) normal pressure is refined: raw material honey being pumped into jacketed pan, jacketed pan steam valve is opened, presss from both sides under constant stirring
Layer is passed through 0.2-0.3Mpa steam, and honey is warming up to 75-85 DEG C, refines 12h, is continuously heating to 105-120 DEG C, boils 2h, closes
5h is placed after closing steam valve；
(3) the screen to filtrate: by the honey after standing through the screen to filtrate, it is then sent to cold boiler；
(4) negative pressure is refined: in cold boiler, in the case where vacuum degree is 0.06-0.07Mpa condition of negative pressure, being concentrated
Photoelectricity refractometer is observed in refining, controls moisture；
(5) honey refined is inputted into storage honey jar.
Embodiment 4
A kind of refined honey method suitable for the production of big honeyed bolus,
(1) raw material selects: selecting faint yellow sticky syrupy shape honey is raw material；
(2) normal pressure is refined: raw material honey being pumped into jacketed pan, jacketed pan steam valve is opened, presss from both sides under constant stirring
Layer is passed through 0.1-0.2Mpa steam, and honey is warming up to 75-85 DEG C, refines 15h, is continuously heating to 105-120 DEG C, boils 1.5h,
15h is placed after steam off valve；
(3) the screen to filtrate: by the honey after standing through the screen to filtrate, it is then sent to cold boiler；
(4) negative pressure is refined: in cold boiler, in the case where vacuum degree is 0.07-0.08Mpa condition of negative pressure, being concentrated
Refining controls moisture；
(5) honey refined is inputted into storage honey jar.
Claims (1)
1. a kind of refined honey method suitable for honeyed bolus, which is characterized in that step are as follows:
(1) raw material selects: using sticky syrupy shape creamy white or light yellow or thick such as congealed fat shape semifluid honey as raw material；
(2) normal pressure is refined: raw material honey being pumped into jacketed pan, jacketed pan steam valve is opened, presss from both sides under constant agitation
Layer is passed through 0.1-0.5Mpa steam, and honey is warming up to 75-85 DEG C, refines 5-15h, is continuously heating to 105-120 DEG C, boils 0.5-
2h stands 5-15h after steam off valve；
(3) the screen to filtrate: by the honey after standing through the screen to filtrate, it is then sent to cold boiler；
(4) negative pressure is refined: in the cold boiler that vacuum degree is 0.04-0.08Mpa, negative pressure concentration refining is rolled over using photoelectricity
Penetrate instrument control moisture；
(5) honey refined is inputted into storage honey jar.
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| CN113390821B (en) * | 2021-05-21 | 2024-04-12 | 北京中医药大学 | Real-time monitoring equipment and method for quality of intelligent honey refining process |
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| RU2407403C1 (en) * | 2009-10-14 | 2010-12-27 | Сергей Викторович Афанасьев | Aqueous solution of honey and its authenticity control method |
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