CN106512018A - Honey refining method suitable for honey boluses - Google Patents
Honey refining method suitable for honey boluses Download PDFInfo
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- 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
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Abstract
The invention discloses a honey refining method suitable for honey boluses. The honey refining method suitable for the honey boluses comprises the steps that (1) honey is selected as a raw material; (2) the raw material honey is sucked into a jacketed kettle, a steam valve of the jacketed kettle is opened, and steam is led into an interlayer under continuous stirring, the honey is heated to 75-85 DEG C, refined for 5-15 h, continuously heated to 105-120 DEG C, decocted for 0.5-2 h, and held for 5-15 h after the steam valve is closed; (3) the stewed honey is filtered through a sieve, and then conveyed to a vacuum evaporator; (4) concentration refining is conducted in the vacuum evaporator under the negative pressure condition, a photoelectric refractometer is observed, and moisture is controlled; and (5) the refined honey is conveyed into a honey storage pot. The honey refining method combines jacketed kettle steam atmospheric pressure heating with vacuum decompression concentration, and is good in stability, low in medical composition loss in the preparation process, high in quality and easy to operate.
Description
Technical field
The present invention relates to a kind of white silk honey method suitable for big honeyed pills.
Background technology
Honeyed pill is a kind of most widely used dosage form of tcm clinical practice, occupies very important status in Chinese medicine preparation.Honey
Ball is stable in properties, carries easy to use, and toxic and side effects are little, as excipient or correctivess in preparation, can relax the property of medicine, increase
The curative effect of medicine, strengthens medicine invigorating the spleen and replenishing QI, effect of nourishing the lung to arrest cough.
Rich in nutrient substance such as abundant sugar, organic acid, vitamin in Mel, relieving asthma with nourishing, laxation, relieving constipation, solution
Poison etc. is acted on.Modern study illustrates that the Mel after processing can strengthen the dissolubility of aglycon in some medical materials in order to absorb, and
Possess reproducibility and anti-corrosive antibacterial effect, the oxidation deterioration of effective ingredient in medical material can be avoided, it is ensured that the quality of medicine.But
It is that Mel contains 25% or so moisture, a portion is moisture inferior, separately has the impurity such as dead honeybee, waxiness, starchy material.
Waxiness can float on pill surface, form very thin wax coat, deposit long and can crack, and when starch-containing class is more, then finished product is dry and cracked.
Therefore, Mel has to pass through refining before ball is entered, and to remove impurity, destroys ferment, kills microorganism, suitably reduce moisture, increases
Plus bonding force.
According to refining temperature and finished product feature, refined honey is divided into tender sweet, middle sweet and old honey, wherein tender sweet heating-up temperature is
105-115 DEG C, water content more than 20%, five significant change of color, slightly stickiness；Middle sweet heating-up temperature is 116-119 DEG C, aqueous
Amount 10%-13%, color have stickiness in faint yellow；Old sweet hot temperature is 119-122 DEG C, and water content is less than 4%, and color is in reddish brown
Color, has strong tack, i.e. the easily restriction of heated method and condition.Thus while having so, clearly data specify, in reality
Do not widely use in the work of border.
Mel refining quality directly affects the quality of sweet inflammation medicine and honeyed pill.If refining is inadequate, honeyed pill is in storage period
Easily there are the quality problems such as elephant skin, mouldy, stiff, rupture, sand return, therefore, need to carry out strictly quality in refining process
Monitoring.Traditional refining fado is refined using normal pressure, i.e., boiling water is added in Mel（Or add water in Mel and boil）, make to dissolve,
And suitably dilute, by three to No. four screen clothes to filter impurity, filtrate is heated in putting copper pot, and constantly skimming, stirring, to needs
Degree.Modern refined honey mainly uses refining temperature as Con trolling index, but still needs to according to prescription Chinese medicine powder water content and Drug
Matter is grasping refining degree.
At present, normal pressure refined honey is heated using jacketed pan steam generally.But due to the ununified technological principle of refined honey and have
The prescription of pass, causes various places enterprise to carry out refined honey using different temperature and times, causes the quality of refined honey uneven,
Easily go out the excessively soft or really up to the mark phenomenon of ready-made article, affect attractive in appearance, or even cause the honeyed pill moisture absorption, go mouldy or hard, or even affect medicine
Product curative effect.According to data, Chinese Pharmacopoeia and the specific Mel of the also no clear stipulaties of each province and city medicinal material processing specification refine work
The quality standard of skill and refined honey, therefore, research and development one kind has the governed honeyed pill refined honey method of quality standard, is urgently to be resolved hurrily at present
Problem.
The content of the invention
The present invention's is really up to the mark or excessively soft, impact quality easily occur for the finished product refining for solving prior art presence
With the problem of curative effect, and provide a kind of good stability, preparation process active ingredient lose low, quality it is high suitable for big
The refined honey method of honeyed pill production.
The present invention is achieved by the following technical solutions：
A kind of refined honey method suitable for big honeyed pills production,
（1）Material choice：Selection Mel is raw material；
（2）Normal pressure is refined：By in raw material Mel suction jacketed pan, jacketed pan steam valve is opened, led to lower interlayer is stirred continuously
Enter steam, Mel is warming up to 75-85 DEG C, refine 5-15h, be continuously heating to 105-120 DEG C, boil 0.5-2h, steam off valve
5-15h is placed behind the door；
（3）Screen filtration：By the Mel Jing screen filtrations after standing, vacuum evaporator is then sent to；
（4）Negative pressure is refined：In vacuum evaporator, under condition of negative pressure, concentration refining is carried out, observe photoelectricity refractometer, control
Moisture；
（5）By the Mel refined input storage honey jar.
Further, milky or faint yellow sticky syrupy shape are selected or thick if lipoid shape semifluid Mel is raw material.
When described normal pressure is refined, 0.1-0.5Mpa steam is passed through under agitation.
When described negative pressure is refined, vacuum is 0.04-0.08Mpa.
It is described to carry out concentration refining under condition of negative pressure, it is controlling moisture by observing photoelectricity refractometer.
The present invention utilizes jacketed pan, the refined honey method combined with vacuum-concentrcted using heating normal pressure, overcomes existing
The finished product that technology is present is really up to the mark or excessively soft, affects the problem of quality and curative effect.Specifically, first, the present invention adopts normal pressure
The refined honey method combined with concentrating under reduced pressure method, non-pressure process control refined honey quality, vacuum-concentrcted method control moisture；Its
Secondary, Mel has a good antioxidant activity after processing, reason be in Mel carbohydrate content (69-86%) based on monosaccharide, wherein
Fructose content accounts for 38%, and glucose content accounts for 31%, and high-temperature heating can make sugar that caramelization, the caramelization of sugar occur
There is product preferable antioxidant activity, 5-HMF, phenols etc. also to have good non-oxidizability, during refined honey of the present invention first
75-85 DEG C of refining is warming up to, this step is generated 5-HMF by overabundant heat cyclodehydration by glucose；After 5-15h, temperature rises to 105-
120 DEG C boil 0.5-2h, and Fructose participates in reaction, and the polyphenol content of generation increases notable, and non-oxidizability strengthens, DPPH clearance rate ratio
First step Fructose, glucose are big more when coexisting, therefore, the 5-HMF generated during refined honey is relatively fewer, and non-oxidizability is aobvious
Write；Again, the rising of the prolongation of heat time heating time, heating-up temperature, the color burn of Mel and antioxidation strengthen, the face of Mel
It is significantly correlated between color and antioxidant activity, but the refined honey time exceed time Mel of the present invention in nutrient substance be lost in
In serious, refined honey loses the meaning originally having；Finally, existing Mel refining process disunity, criteria of quality evaluation lack, and cause refining
Honey quality be difficult control, the present invention on the basis of existing technology, by polyphenol content measure, 5-HMF contents, the measure of pH etc.
Used as the index composition of quality control, and 5-HMF assays make result more accurate using high-efficient liquid phase technique, better control over
Refined honey quality, aldehydes matter are the important activity compositions of Mel, and especially ortho position phenolic hydroxyl group is easily oxidized its phenolic hydroxyl structure
Into quinones structure, the ability with very strong removing free radical.Polyphenol can be big with protein (enzyme), polysaccharide, alkaloid and biology
Molecule compound reaction, adds the activity of its own removing free radical having so as to more physiologically active, such as anti-to lure
Become, anti-ageing wait for a long time.Polyphenol content is the strong and weak important criterion of Mel activity, it may be possible to which before and after affecting Mel refining, the property of medicine changes
The key of change, 5-HMF are not present in fresh Mel, and with being continuously increased in processing or ageing process.5-HMF is affected to contain
The factor of amount has much, such as temperature and heat time heating time, pH, Hua Yuan etc., therefore 5-HMF contents can be used as superheated detection
Index.
In refining process of the present invention, strict quality control to be carried out to refined honey：
（1）Sample preparation：When refining in aforementioned manners, sample 50g is taken at interval of 25 DEG C, each temperature spot takes wherein 2g to examination
Pipe, distills water dissolution and is settled to 25ml, and 4000rpm is centrifuged 20 minutes, takes supernatant, obtains the honey sample of 80mg/ml, be used for
Analysis physicochemical property.
（2）Total phenol content is determined：Total phenol content is determined using Folin-Ciocalteu methods, solution and reference substance is prepared
The compound method of the sodium carbonate liquor of solution, wherein 1mol/L is that precision weighs 21.2g natrium carbonicum calcinatums, distills water dissolution, fixed
Hold 200mL, shake up and obtain final product；The preparation of gallic acid reference substance solution is that precision weighs 10mg gallic acid reference substances, with steaming
Simultaneously constant volume, to 10mL, shakes up and obtains final product 1.0mg/mL gallic acid reference substance storing solutions for distilled water dissolving；Take storing solution appropriate, it is dilute with water
It is interpreted into the series standard solution that concentration is 5,10,25,50,80,100 g/mL；
Concrete assay method is as follows：Take 100 L honey samples（80mg/mL）Or gallic acid standard solution, plus l00 L
Folin-Ciocalteu developers, after mixing, plus the sodium carbonate liquor of 0.5mL mol/L, 300 L of distilled water, in room temperature, keep away
1h is placed under optical condition, the mensuration absorbance under 760nm.
（3）5-HMF assays：
The preparation of reference substance solution：First 0.011g 5-HMF standard substance are dissolved, constant volume is configured to 1.1mg/mL former to 10mL
Liquid, then it is diluted with water to the series standard solution of 0.011,0.022,0.11,0.22,1.1,11,22 g/mL；
The pretreatment of sample：Take honey sample, 8 times of dilute with water, with 0.45 m filtering with microporous membranes, gained filtrate uses HPLC
Detected；
Chromatographic condition：Chromatographic column：C18(150mm × 4.6mm, 5 m) for chromatographic column；Mobile phase：Acetonitrile：0.1% phosphoric acid solution=4:
92；Column temperature：25℃；Detection wavelength：Wavelength 284nm；Flow velocity：1mL/min；Sample size：20µL；Accurate absorption standard substance are molten respectively
Liquid and each 20 L of sample solution, inject chromatograph of liquid, determine, obtain final product.
（4）Colour measurement：Determined by absorbance of the 80mg/ml honey samples at 420nm.
（5）Acid-base value is determined：Determined by PH meters.
In order to verify effect of the present invention, to carrying out quality determination according to finished product obtained in this inventive method
1st, total phenol content is determined
（1）The drafting of gallic acid standard curve
In Mel, the measure of total phenol content is, as standard, to be determined using Folin-Ciocalteu methods, not have with gallic acid
Gallate-based concentration C（µg/mL）For abscissa, the absorbance A at 760nm maps for vertical coordinate, as shown in figure 1, the data obtained
As shown in table 1, linear regression treatment obtains calibration curve equation：A=0.23926x-0.21207, R2=0.99011, in 5 g/
It is linear between the g/mL of mL to 100.
1 gallic acid standard curve of table
（2）Sample total phenol content measurement result
In Mel refining process, TPC is calculated according to gallic acid standard curve, and content range is in the g/ of 90.84 g/g to 1236.28
Between g, 14 times are increased, as shown in Fig. 2 result is as shown in table 2, figure it is seen that with the rising of refined honey temperature, always
Phenol content is constantly raised, and when 125 DEG C or so, elevation amplitude is gradually steady.
Total phenol content change in 2 Mel refining process of table
2nd, 5-HMF assays result
（1）Specificity is analyzed：Under measure chromatographic condition, 5-HMF peak shapes are good, with other chromatographic peak separating degrees in sample liquid
Well, 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, RSD values are calculated for 0.95% (n=6), bat is
100.19%, illustrate that lower limit of quantitation meets sample determination requirement.
3 lower limit of quantitation of table (0.1100 g/mL) investigates result data (n=6)
（3）Linear relationship is investigated
The measure of 5-HMF reference substance solution standard curves as shown in figure 5, result as shown in table 4, standard curve regression equation is：A
=145.1C-2.7313, R2=0.99992,5-HMF concentration in the range of 0.0110 ~ 22 g/mL, linear relationship is good.
4 5-HMF standard curves of table
（4）Precision measurement result
According to the measure concentration and the degree of closeness of theoretical actual concentration of 5-HMF reference substance solution, the precision of method is investigated.Survey
Determine result see the table below.
5 precision data result of table
Precision RSD value is 1.43% (n=6), and bat is 98.73%, as a result shows that the method precision meets the requirements.
（5）Repeated measurement result
The measurement result of repeated experiment is shown in Table 6, RSD values for 0.40%.Illustrate that the method repeatability result meets inspection requirements.
6 method of table repeatability data result（n=5）
（6）Stability Determination result
Stability Determination the results are shown in Table 7, and with sample, the measure concentration of 5-HMF contents calculates RSD values as 0.2%, illustrates detected sample
Product are stable in 24 hours.
7 stability test data result of table
| Time（h） | 0 | 1 | 2 | 4 | 8 | 12 | 24 | Average | 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 reclaims measurement result
The measurement result of sample-adding recovery experiment is shown in Table 8, and average recovery rate is that 99.3620%, RSD values are 0.76%, illustrates the measure
Method reliability.
Table 8 is loaded recovery experiment test data result（n=5）
3rd, colour measurement result
In Mel refining process, color change measurement result is shown in Table 9,
Color change in 9 Mel refining process of table（80mg/mL）
As a result show that Mel color intensity after processing through processing has significant change.
4th, Acidity of Aikalinity measurement result
The pH value of the refining Mel determined under different temperatures is as shown in table 10,
PH value change in 10 Mel refining process of table（80mg/mL）
| 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, in Mel refining process the scope of pH value change between 3.77 to 4.15, in the 75min at the initial stage of processing
In pH value rise to 4.15 from 3.95, again drop to 3.77 during 75min to 150min.There are early stage pH risings in honey sample
The reason for be probably in Mel original some acidic materials caused by thermal response decomposition, the reduction of later stage pH value is probably then
Due to occurring what the degraded such as nonenzymatic browning reaction and Fructose was caused.
Compared with prior art, the present invention heats the method white silk combined with vacuum-concentrcted by normal pressure using jacketed pan steam
Honey, good stability, it is high, simple to operate that preparation process active ingredient loses low, quality.
Description of the drawings
Fig. 1 is gallic acid canonical plotting；
Fig. 2 is total phenol content change in refining process；
Fig. 3 is schemed for reference substance 5-HMF；
Fig. 4 is 100 minutes Mel 5-HMF figures of refining；
Fig. 5 is 5-HMF canonical plottings.
Specific embodiment
The invention will be further described with reference to embodiments.
Embodiment 1
A kind of refined honey method suitable for big honeyed pills production,
（1）Material choice：The sticky syrupy shape Mel of milky is selected to be raw material；
（2）Normal pressure is refined：By in raw material Mel suction jacketed pan, jacketed pan steam valve is opened, led to lower interlayer is stirred continuously
Enter 0.4-0.5Mpa steam, Mel is warming up to 75-85 DEG C, refine 5h, be continuously heating to 105-120 DEG C, boil 1h, steam off
12h is placed after valve；
（3）Screen filtration：By the Mel Jing screen filtrations after standing, vacuum evaporator is then sent to；
（4）Negative pressure is refined：In vacuum evaporator, it is, under 0.04-0.05Mpa condition of negative pressure, to carry out concentration refining in vacuum,
Control moisture；
（5）By the Mel refined input storage honey jar.
Embodiment 2
A kind of refined honey method suitable for big honeyed pills production,
（1）Material choice：Select thick if lipoid shape semifluid Mel is raw material；
（2）Normal pressure is refined：By in raw material Mel suction jacketed pan, jacketed pan steam valve is opened, led to lower interlayer is stirred continuously
Enter 0.3-0.4Mpa steam, Mel is warming up to 75-85 DEG C, refine 8h, be continuously heating to 105-120 DEG C, boil 0.5h, close and steam
Steam valve places 8h behind the door；
（3）Screen filtration：By the Mel Jing screen filtrations after standing, vacuum evaporator is then sent to；
（4）Negative pressure is refined：In vacuum evaporator, it is, under 0.05-0.06Mpa condition of negative pressure, to carry out concentration refining in vacuum,
Observation photoelectricity refractometer, controls moisture；
（5）By the Mel refined input storage honey jar.
Embodiment 3
A kind of refined honey method suitable for big honeyed pills production,
（1）Material choice：The sticky syrupy shape Mel of milky is selected to be raw material；
（2）Normal pressure is refined：By in raw material Mel suction jacketed pan, jacketed pan steam valve is opened, led to lower interlayer is stirred continuously
Enter 0.2-0.3Mpa steam, Mel is warming up to 75-85 DEG C, refine 12h, be continuously heating to 105-120 DEG C, boil 2h, close and steam
Steam valve places 5h behind the door；
（3）Screen filtration：By the Mel Jing screen filtrations after standing, vacuum evaporator is then sent to；
（4）Negative pressure is refined：In vacuum evaporator, it is, under 0.06-0.07Mpa condition of negative pressure, to carry out concentration refining in vacuum,
Observation photoelectricity refractometer, controls moisture；
（5）By the Mel refined input storage honey jar.
Embodiment 4
A kind of refined honey method suitable for big honeyed pills production,
（1）Material choice：Faint yellow sticky syrupy shape Mel is selected to be raw material；
（2）Normal pressure is refined：By in raw material Mel suction jacketed pan, jacketed pan steam valve is opened, led to lower interlayer is stirred continuously
Enter 0.1-0.2Mpa steam, Mel is warming up to 75-85 DEG C, refine 15h, be continuously heating to 105-120 DEG C, boil 1.5h, close
15h is placed after steam valve；
（3）Screen filtration：By the Mel Jing screen filtrations after standing, vacuum evaporator is then sent to；
（4）Negative pressure is refined：In vacuum evaporator, it is, under 0.07-0.08Mpa condition of negative pressure, to carry out concentration refining in vacuum,
Control moisture；
（5）By the Mel refined input storage honey jar.
Claims (5)
1. a kind of refined honey method suitable for honeyed pill, it is characterised in that step is：
（1）Material choice：Selection Mel is raw material；
（2）Normal pressure is refined：By in raw material Mel suction jacketed pan, jacketed pan steam valve is opened, led to lower interlayer is stirred continuously
Enter steam, Mel is warming up to 75-85 DEG C, refine 5-15h, be continuously heating to 105-120 DEG C, boil 0.5-2h, steam off valve
5-15h is stood behind the door；
（3）Screen filtration：By the Mel Jing screen filtrations after standing, vacuum evaporator is then sent to；
（4）Negative pressure is refined：In vacuum evaporator, under condition of negative pressure, concentration refining is carried out, control moisture；
（5）By the Mel refined input storage honey jar.
2. the refined honey method suitable for honeyed pill according to claim 1, it is characterised in that described raw material be milky or
Faint yellow sticky syrupy shape, or it is thick such as lipoid shape semifluid Mel.
3. the refined honey method suitable for honeyed pill according to claim 1 and 2, it is characterised in that when described normal pressure is refined,
0.1-0.5Mpa steam is passed through under agitation.
4. the refined honey method suitable for honeyed pill according to claim 1 and 2, it is characterised in that when described negative pressure is refined,
Vacuum is 0.04-0.08Mpa.
5. the refined honey method suitable for honeyed pill according to claim 1 and 2, it is characterised in that described moisture Control, be
Observation control is carried out using photoelectricity refractometer.
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| CN201611099923.2A CN106512018B (en) | 2016-12-05 | 2016-12-05 | A kind of refined honey method suitable for honeyed bolus |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110292163A (en) * | 2019-07-29 | 2019-10-01 | 浙江中医药大学 | A kind of constant temperature refined honey method |
| CN113390821A (en) * | 2021-05-21 | 2021-09-14 | 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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2016
- 2016-12-05 CN CN201611099923.2A patent/CN106512018B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2407403C1 (en) * | 2009-10-14 | 2010-12-27 | Сергей Викторович Афанасьев | Aqueous solution of honey and its authenticity control method |
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| 毛淑杰等: ""中药炮制辅料——蜂蜜古今炼制工艺及标准"", 《科技创新导报》 * |
| 王凤翔等: ""减压和常压炼蜜对蜂蜜成分的影响"", 《中成药研究》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110292163A (en) * | 2019-07-29 | 2019-10-01 | 浙江中医药大学 | A kind of constant temperature refined honey method |
| CN113390821A (en) * | 2021-05-21 | 2021-09-14 | 北京中医药大学 | Real-time monitoring equipment and method for quality of intelligent honey refining process |
| 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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| CN106512018B (en) | 2019-09-24 |
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