CN106770695A - The quality standard and manufacturing process of the bark of eucommia qualitative, quantitative prepared slices of Chinese crude drugs - Google Patents
The quality standard and manufacturing process of the bark of eucommia qualitative, quantitative prepared slices of Chinese crude drugs Download PDFInfo
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- CN106770695A CN106770695A CN201610368303.8A CN201610368303A CN106770695A CN 106770695 A CN106770695 A CN 106770695A CN 201610368303 A CN201610368303 A CN 201610368303A CN 106770695 A CN106770695 A CN 106770695A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/46—Eucommiaceae (Eucommia family), e.g. hardy rubber tree
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/13—Preparation or pretreatment of starting material involving cleaning, e.g. washing or peeling
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/17—Preparation or pretreatment of starting material involving drying, e.g. sun-drying or wilting
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
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Abstract
The invention provides one kind is safe efficient, the easily bark of eucommia prepared slices of Chinese crude drugs.The bark of eucommia qualitative, quantitative prepared slices of Chinese crude drugs manufacturing process that the present invention is provided, using a kind of processing procedure, the bark of eucommia that quality standard will be met is prepared into the prepared slices of Chinese crude drugs, can brew and take change traditional decoction instructions of taking, while providing a kind of bark of eucommia quality standard, coherent detection project be increased on the basis of existing quality standard, and improve the standard limits of Pinoresinol diglucoside in assay, quality that can be effectively to the bark of eucommia is controlled, and improves the quality standard of medicine, increased drug safety.
Description
Technical field
The present invention relates to the field of Chinese medicines, the specially quality standard of the bark of eucommia qualitative, quantitative prepared slices of Chinese crude drugs, operational procedure and system
Make technique.
Background technology
The bark of eucommia (scientific name：Eucommia μ lmoides Oliv) silk flosssilk wadding skin, silk gross weight are called, it is the distinctive seeds of China.
The bark of eucommia as conventional Chinese medicine, with powerful potentiality to be exploited.The bark of eucommia is rich in gutta-percha, glucoside-containing, alkaloid, pectin, fat, tree
The active ingredients such as fat, organic acid, ketose, its function is with to cure mainly be filling liver kidney, and strengthening the bones and muscles is antiabortive.For kidney deficiency and liver, waist and knee acid
Bitterly, muscles and bones is powerless, has a dizzy spell, blood leaking in gestation, fetal irritability.Bark of eucommia tradition concocting method uses scrubbing brush brush to be put into clear water
Dust or soil scrape off tertia, pick up and are filtered dry moisture content, upper lid wet cloth, moisten for 1 night, and six points of panes are cut in taking-up, dry or dry.
Take it and fry (10 grams of change water of pharmaceutical salts per jin) by medicine input pot with salt solution, with frying with salt solution is spilt, it is degree to fry to band black fracture of wire.
Traditional decoction takes more time and effort consuming, therefore brews the bark of eucommia prepared slices of Chinese crude drugs taken in the urgent need to a kind of.
The prepared slices of Chinese crude drugs are the parts that Chinese medicine industry can not be lacked, and being that tcm clinical practice is dialectical treats required tradition force
Device, the curative effect that its quality directly affects tcm clinical practice diseases prevention, cures the disease, otherwise for the quick rhythm of life of modern, the present invention
The high-quality of offer, can brew take change traditional decoction instructions of taking the prepared slices of Chinese crude drugs have the larger market demand.
Problem to be solved by this invention is that the generally existing prepared slices of Chinese crude drugs curative effect for solving in the market is not obvious, Chinese medicine
Process and formulation, the compatibility of Chinese medicine, dosage, method of administration, the factor such as allotment, decoction method, diet of Chinese medicine is to Chinese Herbs
Have a significant effect.(the factor of Liu Hongxing, fourth tree simple analysis influence Chinese Herbs【J】Traditional Chinese medicine, 2014).Growth of Eucommia ulmoides
In main disease have damping-off, root rot, leaf blight, the agricultural chemicals used in controlling disease is also easy to produce the matter such as residues of pesticides are exceeded
Amount problem (generation of burnt open-birth bark of eucommia Major Diseases and preventing and treating【J】Plant protection, 2015).By to bark of eucommia heavy metal unit
The research of plain enriched character, as a result shows that folium cortex eucommiae and the Pb constituent contents of skin easily exceed forestry industry sanitary standard, and its is right
The height of the comprehensive accumulation ability of heavy metal element (As, Pb, Hg, Cd) there is also difference (the barks of eucommia such as Chen Dewen heavy metal unit
Plain enrichment characteristics research【J】Research and discussion, 2007).Heavy-metal residual detection is particularly important.
Brief description of the drawings
Accompanying drawing 1 is bark of eucommia qualitative, quantitative Manufacture of medicinal slices of TCM process chart.
The content of the invention
In order to solve the above problems, quality standard and the manufacture work of the bark of eucommia qualitative, quantitative prepared slices of Chinese crude drugs that the present invention is provided
Skill, increases to medicine bits impurity, heavy metal and harmful element, Residual Levels of Organochlorine Pesticides, AFB1, sulfur dioxide residue
The detection of amount, and the standard limits of the Pinoresinol diglucoside in assay are improved to 0.11% from 0.10%.And lead to
Cross specific operation and produce the bark of eucommia prepared slices of Chinese crude drugs, it is ensured that the prepared slices of Chinese crude drugs meet high standard quality requirements.
The manufacturing process of the bark of eucommia qualitative, quantitative prepared slices of Chinese crude drugs that the present invention is provided, comprises the following steps：
A10, net system：The impurity that is mixed in the bark of eucommia of removing and the product that go mouldy etc., to reach clean or to be processed further treatment.
Note：The bark of eucommia must not directly contact ground after cleaning.
A20, demulcen：The bark of eucommia after net system is put into Xi Run ponds, water spray heap profit 16-24h, is thoroughly run through to the bark of eucommia.Note：
The bark of eucommia need to run through, soft or hard suitable inside and outside the bark of eucommia.
A30, remove tertia：The bark of eucommia that will be run through removal tertia.
A40, cutting：Broken 0.3~1mm.Operated by fully automatic high-speed slicer operational procedure, mix up knife away from the bark of eucommia is entered
Row trial cut, is detected with slide measure, adjusts cutting width, formally cuts medicine after meeting the requirements again.
A50, drying：It is dried using heated-air circulation oven, the bark of eucommia is laid on baking oven shelf, paving thickness is uniform,
Thickness is in below 3cm.Switch is opened, heater switch, blower fan is opened, 60 ± 2 DEG C are dried in temperature, and setting is reached in temperature
6-8h is dried after temperature, drying is finished, and closes heater switch, continue to dry, treat that the temperature inside the box is fallen to 35~40 DEG C, close wind
Machine.Post personnel need to fill in intermediate products and please examine list after drying, hand over Quality Mgmt Dept to carry out moisture inspection by QA samplings.
A60, packaging：Packed according to the requirement of this product packing specification.Need to check make-up room before packaging, confirm bag
Clearing out a gathering place for assembling production lines has been completed, and checks whether packaging material meet the requirements.Inner packing：Being adjusted in equipment needs print
The date of manufacture of system, lot number, QA monitoring, the bark of eucommia for weighing predetermined weight are put into hopper, are sealed with sealing machine, it is desirable to accomplish envelope
Mouth is tight, smooth, attractive in appearance.External packing：Adjusted in equipment the date of manufacture and lot number that need to be printed, QA monitoring, in external packing
Lot number, date of manufacture are printed on box, should be noted whether lot number and date of manufacture are clear in print procedure.After the completion of inner packing
Medicine materical crude slice and survey report be put into outsourcing box, 4 bags/box.Every 10 box medicine materical crude slice is inserted in 1 heat shrinkage film, carries out hot receipts
Contracting；It is fitted into after thermal contraction in big carton, 240 boxes/case.In operating process, QA is inspected by random samples at any time.Post personnel need to fill in into after packaging
Product please examine list, hand over Quality Mgmt Dept to carry out product examination by QA samplings.
A70, finished product：Post personnel need to fill in finished product and please examine list after packaging, hand over Quality Mgmt Dept to carry out product examination by QA samplings.
Increase to medicine bits impurity, heavy metal and harmful element, Residual Levels of Organochlorine Pesticides, AFB1, titanium dioxide
The detection of sulphur residual quantity, and by the standard limits of the Pinoresinol diglucoside in assay from 0.10% improve to
0.11%.The quality standard of the revised bark of eucommia qualitative, quantitative prepared slices of Chinese crude drugs is as follows：
Bark of eucommia medicine materical crude slice
Phonetic title：Duzhong Yinpian
Packaging：Fine aluminium composite film packaging.
Proterties
Take this product appropriate, observe in the sunlight, in thread, outer surface light brown or taupe have obvious wrinkle to this product.
Section has fine and closely woven, silvery white, rubber thread full of elasticity to be connected.It is smelt, gas is micro-, taste it, taste is slightly bitter.
Differentiate
Microscopical characters
Instrument and apparatus：Medicinal herb grinder, pharmacopeia sieve, microscope, alcolhol burner
Reagent and test solution：(reagent is used and divided for chloraldurate test solution, glycerine acetic acid test solution, glycerol-alcohol test solution, dilute glycerine
Analysis is pure, and experimental water is purified water)
Determine and result judgement：In right amount, picking is put on slide a little, and glycerine vinegar is added dropwise to take this product powder (crossing No. four sieves)
Sour test solution, chloraldurate test solution or other test solutions 1~2 drop, covered.After chloraldurate test solution is added dropwise if necessary, in wine
Saturatingization is heated on smart lamp, and glycerol-alcohol test solution or dilute glycerine, covered, in basis of microscopic observation is added dropwise：This product powder
Brown.Rafter collodion silk is agglomerating into bar or distortion, and surface shows graininess.Lithocyte is a lot of, mostly in groups, rectangle like, similar round, length
Bar shaped is in irregular shape, is about to 180 μm, 20~80 μm of diameter, and wall thickness, some cells include rubber agglomerate.Cork cell
Surface sight polygonal, 15~40 μm of diameter, wall is uneven to be thickened, and woodization has tiny pit；Rectangle is seen in side, and the face of wall three increases
Thickness, simultaneously thin, hole ditch is obvious.
Physics and chemistry differentiates
Reagent and test solution：Chloroform, ethanol (reagent is pure using analysis)
Determine and result judgement：This product powder 1g, plus chloroform 10ml are taken, is impregnated 2 hours, filtration.Filtrate volatilizes, plus
Ethanol 1ml, produces the glued membrane of tool elasticity.
Check
Medicine bits, impurity
Instrument and apparatus：Medicinal herb grinder, assay balance, pharmacopeia sieve
Test sample about 100g (being accurate to 0.1g) is taken, is spread out, sort out impurity, sifted out medicine with No. 6 and consider to be worth doing, merged, weighed, counted
Calculate its amount (%) in test sample.
Result judgement：This product medicine bits, impurity must not cross 3%.
Moisture
Instrument and apparatus：Medicinal herb grinder, assay balance, pharmacopeia sieve, electric heating constant-temperature blowing drying box, measuring cup
Determine and result judgement：Determined according to aquametry (method of general rule 0,832 second).
2~5g of test sample is taken, is laid in and is dried into the flat measuring cup of constant weight, thickness is no more than 5mm, loose test sample
Accurately weighed no more than 10mm, open bottle cover covers bottle cap in 100~105 DEG C of dryings 5 hours, in dislocation drier, puts
It is cold 30 minutes, accurately weighed, then dried 1 hour in said temperature, let cool, weigh, it is no more than to the double difference weighed
Untill 5mg.According to the weight of less loss, water content (%) in test sample is calculated.
Result judgement：This product moisture must not cross 13.0%.
Heavy metal and harmful element
Instrument and apparatus：Medicinal herb grinder, assay balance, pharmacopeia sieve, microwave dissolver, atomic absorption spectrophotometer
Reagent and test solution：Nitric acid, ammonium dihydrogen phosphate, magnesium nitrate, KI, ascorbic acid, hydrochloric acid, sodium borohydride, hydrogen-oxygen
(wherein nitric acid, ammonium dihydrogen phosphate, magnesium nitrate are top pure grade, and other reagents are used to change sodium, sulfuric acid, potassium permanganate, hydroxylamine hydrochloride
Analysis is pure, and experimental water is purified water)
Standard sample：Lead single element standard sample, cadmium single element standard sample, arsenic single element standard sample, mercury single element
Standard sample, copper single element standard sample
Method：Determined according to lead, cadmium, arsenic, mercury, copper determination method (general rule 2321)
The measure (graphite furnace method) of lead
Condition determination reference conditions：Wavelength 283.3nm, 100~120 DEG C of drying temperature continues 20 seconds；Ashing temperature 400
~750 DEG C, continue 20~25 seconds；Atomization temperature 1700~~2100 DEG C, continue 4~5 seconds.
The preparation precision of lead Standard Reserving Solution measures lead single element standard liquid in right amount, is diluted with 2% salpeter solution, is made
Per the solution of the μ g of 1ml leaded (Pb) 1, obtain final product (0~5 DEG C of storage).
Precision measures lead Standard Reserving Solution in right amount respectively for the preparation of standard curve, and every 1ml difference is made of 2% salpeter solution
The solution of leaded 0ng, 5ng, 20ng, 40ng, 60ng, 80ng.Precision measures 1ml respectively, precision plus containing 1% ammonium dihydrogen phosphate and
The solution 0.5ml of 0.2% magnesium nitrate, mixes, and precision draws 20 μ l injection graphite furnace atomizers, mensuration absorbance, with extinction
It is ordinate to spend, and concentration is abscissa, draws standard curve.
The preparation A methods of need testing solution take test sample meal 0.5g, accurately weighed, put in politef counteracting tank, plus
3~5ml of nitric acid, mixes, and soaked overnight covers inner cap, screws overcoat, put in suitable Hyperfrequency waves eliminating stove, cleared up (by instrument
What device specified clears up procedure operation).After clearing up completely, cancel solution inner canister and put and be slowly heated on electric hot plate rufous steam and wave
It is most, and continuation is slowly concentrated into 2~3ml, lets cool, and is transferred in 25ml measuring bottles with water, and scale is diluted to, shake up, obtain final product.Same method
While reagent preparation blank solution.
Determination method precision measures blank solution and each 1ml of need testing solution, and precision adds and contains 1% ammonium dihydrogen phosphate and 0.2%
The solution 0.5ml of magnesium nitrate, mixes, precision 10~20 μ l of absorption, method mensuration absorbance under the preparation of sighting target directrix curve, from
The content of lead (Pb) in need testing solution is read on standard curve, is calculated, obtained final product.
Cadmium detrmination (graphite furnace method)
Condition determination reference conditions：Wavelength 228.8nm, 100~120 DEG C of drying temperature continues 20 seconds；Ashing temperature 300
~500 DEG C, continue 20~25 seconds；1500~1900 DEG C of atomization temperature, continues 4~5 seconds.
The preparation precision of cadmium Standard Reserving Solution measures cadmium single element standard liquid in right amount, is diluted with 2% salpeter solution, is made
The solution containing the μ g of cadmium (Cd) 1 per 1ml, obtains final product (0~5 DEG C of storage).
Precision measures cadmium Standard Reserving Solution in right amount respectively for the preparation of standard curve, is diluted with 2% salpeter solution and is made every 1ml
The solution of 0ng containing cadmium, 0.8ng, 2.0ng, 4.0ng, 6.0ng, 8.0ng respectively.Accurate respectively to draw 10 μ l, injection graphite furnace is former
Sonization device, mensuration absorbance, with absorbance as ordinate, concentration is abscissa, draws standard curve.
The preparation of need testing solution determines the preparation of need testing solution under item with lead.
Determination method is accurate to draw blank solution and each 10~20 μ l of need testing solution, method under the preparation of sighting target directrix curve
Mensuration absorbance (if test sample has interference, precision can measure standard liquid, blank solution and each 1ml of need testing solution, essence respectively
Solution 0.5ml close plus containing 1% ammonium dihydrogen phosphate and 0.2% magnesium nitrate, mixes, and determines in accordance with the law), read from standard curve and supplied
The content of cadmium (Cd) in test sample solution, calculates, and obtains final product.
The measure (hydride method) of arsenic
Condition determination uses suitable hydride generation system, and (use is faced with containing sodium borohydride and 0.3% sodium hydroxide solution
Preceding preparation) used as reducing agent, hydrochloric acid solution (1 → 100) is carrier fluid, nitrogen is carrier gas, and Detection wavelength is 193.7nm.
The preparation precision of arsenic Standard Reserving Solution measures arsenic single element standard liquid in right amount, is diluted with 2% salpeter solution, is made
The solution containing the μ g of arsenic (As) 1 per 1ml, obtains final product (0~5 DEG C of storage).
Precision measures arsenic Standard Reserving Solution in right amount respectively for the preparation of standard curve, is diluted with 2% salpeter solution and is made every 1ml
The solution of 0ng containing arsenic, 5ng, 10ng, 20ng, 30ng, 40ng respectively.Precision measures 10ml respectively, in putting 25ml measuring bottles, plus
25% liquor kalii iodide (prepared before use) 1ml, shakes up, plus 10% ascorbic acid solution (prepared before use) 1ml, shakes up, and uses
Hydrochloric acid solution (20 → 100) is diluted to scale, shakes up, close plug, puts in 80 DEG C of water-baths and heats 3 minutes, takes out, and lets cool.Take in right amount,
Suction hydride generation system, determines absorption value, and with peak area (or absorbance) as ordinate, concentration is abscissa, draws mark
Directrix curve.
The preparation of need testing solution is prepared with the A methods in the preparation of need testing solution under lead measure item.
Determination method is accurate to draw blank solution and each 10ml of need testing solution, under the preparation of sighting target directrix curve, from " plus
25% liquor kalii iodide (prepared before use) 1ml " rises, and determines in accordance with the law.The arsenic (As) from need testing solution is read on standard curve
Content, calculate, obtain final product.
The measure (cold steam absorption process) of mercury
Condition determination uses suitable hydride generation system, with molten containing 0.5% sodium borohydride and 0.1% NaOH
Used as reducing agent, hydrochloric acid solution (1 → 100) is carrier fluid to liquid (prepared before use), and nitrogen is carrier gas, and Detection wavelength is 253.6nm.
The preparation precision of mercury Standard Reserving Solution measures mercury single element standard liquid in right amount, is diluted with 2% salpeter solution, is made
Per the solution of the μ g of 1ml mercurous (Hg) 1, obtain final product (0~5 DEG C of storage).
The preparation of standard curve respectively precision measure mercury Standard Reserving Solution 0ml, 0.1ml, 0.3ml, 0.5ml, 0.7ml,
0.9ml, in putting 50ml measuring bottles, plus 20% sulfuric acid solution 10ml, 5% liquor potassic permanganate 0.5ml, shake up, 5% hydrochloric acid is added dropwise
Hydroxylamine solution to aubergine just disappears, and is diluted with water to scale, shakes up.Appropriate, suction hydride generation system is taken, is determined and is absorbed
Value, with peak area (or absorbance) as ordinate, concentration is abscissa, draws standard curve.
The preparation A methods of need testing solution take test sample meal 0.5g, accurately weighed, put in polytetrafluoroethylene (PTFE) counteracting tank, plus
3~5ml of nitric acid, mixes, and soaked overnight covers inner cap, screws overcoat, puts in suitable Hyperfrequency waves eliminating stove and cleared up (by instrument
What device specified clears up procedure operation).After clearing up completely, cancel solution inner canister and put on electric hot plate, rufous is slowly heated in 120 DEG C
Steam is waved to the greatest extent, and continues to be concentrated into 2~3ml, is let cool, plus 20% sulfuric acid solution 2ml, 5% liquor potassic permanganate 0.5ml, is shaken up,
5% hydroxylamine hydrochloride solution to aubergine is added dropwise just to disappear, is transferred in 10ml measuring bottles, wash container with water, washing lotion is incorporated in measuring bottle
In, and scale is diluted to, and shake up, it is centrifuged if necessary, supernatant is taken, obtain final product.With method while reagent preparation blank solution.
Determination method is accurate to draw that blank solution is appropriate with need testing solution, the method under sighting target directrix curve preparation determine from
The content of mercury (Hg) in need testing solution is read on standard curve, is calculated, obtained final product.
Cupper determination (flame method)
Condition determination Detection wavelength is 324.7nm, using Air-acetylene Flame, background correction is carried out if necessary.
The preparation precision of copper Standard Reserving Solution measures copper single element standard liquid in right amount, is diluted with 2% salpeter solution, is made
Solution per 1ml cupric (Cu) 10 μ g, obtains final product (0~5 DEG C of storage).
Precision measures copper Standard Reserving Solution in right amount respectively for the preparation of standard curve, and every 1ml difference is made of 2% salpeter solution
The μ g of cupric 0,0.05 μ g, 0.2 μ g, 4 μ g, 0.6 μ g, the solution of 0.8 μ g.Flame is sprayed into successively, and mensuration absorbance is with absorbance
Ordinate, concentration is abscissa, draws standard curve.
The preparation of need testing solution determines the preparation of need testing solution under item with lead.
Determination method is accurate to draw blank solution with need testing solution in right amount, and the method under the preparation of sighting target directrix curve is surveyed
It is fixed.The content of copper (Cu) from need testing solution is read on standard curve, calculates, and obtains final product.
Result judgement：This product is leaded must not cross 8mg/kg, cadmium must not cross 0.8mg/kg, arsenic must not cross 4mg/kg, mercury must not
Crossing 0.8mg/kg, copper must not cross 20mg/kg.
Organic chlorine agriculture chemicals residual quantity
Instrument and apparatus：Medicinal herb grinder, assay balance, pharmacopeia sieve, Rotary Evaporators, supersonic wave cleaning machine, gas phase color
Spectrometer
Reagent and test solution：Petroleum ether (60~90 DEG C), acetone, sodium chloride, dichloromethane, anhydrous sodium sulfate (its petrochina
(60~90 DEG C) of ether is chromatographically pure, and other reagents are pure using analysis, and experimental water is purified water)
Reference substance：α-BHC, β-BHC, γ-BHC, δ-BHC, p, p '-DDE, p, p '-DDD, o, p '-DDT, p, p '-DDT,
PCNB agricultural chemical reference substances
Method：Determined according to persticide residue determination method (method of general rule 0,512 first).
Chromatographic condition is with system suitability with (14%- cyanogen propvl-phenvl) methyl polysiloxane or (5% phenyl) first
Based polysiloxane is the fused-silica capillary column (30m × 0.32mm × 0.25 μm) of fixer, the capture inspection of 63Ni-ECD electronics
Survey device.230 DEG C of injector temperature, 300 DEG C of detector temperature, Splitless injecting samples.Temperature programming：Initial 100 DEG C, 10 DEG C per minute
220 DEG C are risen to, 8 DEG C per minute rise to 250 DEG C, are kept for 10 minutes.Number of theoretical plate is calculated by α-BHC peaks and should be not less than 1 × 106,
The separating degree of two adjacent chromatographic peaks should be greater than 1.5.
The preparation precision of reference substance stock solution weighs BHC (BHC) (α-BHC, β-BHC, γ-BHC, δ-BHC), drop
DDT (DDT) (p, p '-DDE, p, p '-DDD, o, p '-DDT, p, p '-DDT) and pentachloronitrobenzene (PCNB) agricultural chemical reference substance are suitable
Amount, solution of every 1ml containing about 4~5 μ g is respectively prepared with petroleum ether (60~90 DEG C), is obtained final product.
The preparation precision for mixing reference substance stock solution measures above-mentioned each reference substance stock solution 0.5ml, in putting 10ml measuring bottles,
Scale is diluted to petroleum ether (60~90 DEG C), is shaken up, obtained final product.
The preparation precision of mixed reference substance solution measures above-mentioned mixing reference substance stock solution, with (60~90 DEG C) systems of petroleum ether
Contain the solution of 0 μ g, 1 μ g, 5 μ g, 10 μ g, 50 μ g, 100 μ g, 250 μ g respectively into every 1L, obtain final product.
The preparation of need testing solution takes test sample, is ground into powder (crossing No. three sieves), takes about 2g, accurately weighed, puts 100ml
In conical flask with cover, add water 20ml soaked overnights, and precision adds acetone 40ml, and weighed weight ultrasonically treated 30 minutes, lets cool, then
Weighed weight, supplies the weight of less loss with acetone, then adds sodium chloride about 6g, and precision adds methylene chloride 30ml, weighed weight, ultrasound
15 minutes, then weighed weight, the weight of less loss is supplied with dichloromethane, stand (making layering), organic phase is moved into rapidly and is equipped with
In the 100ml conical flask with cover of appropriate anhydrous sodium sulfate, place 4 hours.Precision measures 35ml, in concentrated under reduced pressure in 40 DEG C of water-baths
To near dry, plus a small amount of petroleum ether (60~90 DEG C) as it is preceding operate repeatedly it is cleared to dichloromethane and acetone, with petroleum ether (60~90
DEG C) dissolve and be transferred in 10ml tool plug graduated centrifuge tubes, plus petroleum ether (60~90 DEG C) precision is diluted to 5ml, is carefully added into
Sulfuric acid 1ml, shakes 1 minute, centrifugation (3000 revs/min) 10 minutes, and precision measures supernatant 2ml, puts the concentrate bottle of tool scale
In, rotary evaporator is connected, be concentrated into solution in right amount by (or using nitrogen) at 40 DEG C, and precision is diluted to 1ml, obtains final product.
Determination method is accurate respectively to be drawn need testing solution and corresponds each 1 μ l of mixed reference substance solution of concentration, note
Enter gas chromatograph, by 9 kinds of Residual Levels of Organochlorine Pesticides in external standard method calculating test sample.
Result judgement：This product (α-BHC, β-BHC, γ-BHC, δ-BHC sums) containing total BHC must not cross 0.2mg/kg；
Total DDT (pp '-DDE, pp '-DDD, op '-DDT, pp '-DDT sums) must not cross 0.2mg/kg；Pentachloronitrobenzene must not mistake
0.1mg/kg。
AFB1
Instrument and apparatus：Medicinal herb grinder, assay balance, pharmacopeia sieve, homogeneous bottle, centrifuge, high performance liquid chromatograph (are matched somebody with somebody
Put fluorescence detector and derivatization pump, derivatization incubator)
Reagent and test solution：(wherein acetonitrile is chromatographically pure, and other reagents are for methyl alcohol, acetonitrile, iodine, sodium chloride, immune affinity column
Analysis is pure, and experimental water is purified water)
Reference substance：AFB1Reference substance
Method：Determined according to aflatoxin determination method (general rule 2351).
Chromatographic condition is with system suitability with octadecylsilane chemically bonded silica as filler；With methanol-acetonitrile-water
(40: 18: 42) are mobile phase；Detected using post-column derivation method, iodine derivatization method：Derivative solution is that 0.05% iodine solution (takes iodine
0.5g, adds methyl alcohol 100ml to make dissolving, is diluted with water to 1000ml and is made), derivatization flow rate pump 0.3ml per minute, derivatization
Temperature 70 C is with fluorescence detector detection, excitation wavelength lambda ex=360nm (or 365nm), emission wavelength lambda ex=450nm.Two
The separating degree of adjacent chromatographic peak should be greater than 1.5.
The preparation precision of mixed reference substance solution measures AFB1(sign concentration is 1.0 μ g/ to reference substance solution
Ml) 0.5ml, in putting 10ml measuring bottles, with methanol dilution to scale, as stock solution.Precision measures stock solution 1ml, puts
In 25ml measuring bottles, with methanol dilution to scale, obtain final product.
The preparation of need testing solution takes test sample powder about 15g (crossing No. two sieves), accurately weighed, is placed in homogeneous bottle, plus
Enter sodium chloride 3g, precision adds 70% methanol solution 75ml, 2 minutes (mixing speed is more than 11000 revs/min) of high-speed stirred,
5 minutes (2500 revs/min of centrifugal speed) of centrifugation, precision measures supernatant 15ml, puts in 50ml measuring bottles, is diluted with water to quarter
Degree, shakes up, and with (0.45 μm) filtration of miillpore filter, measures subsequent filtrate 20.0ml, by immune affinity column, flow velocity 3ml per minute,
Eluted with water 20ml, eluent is discarded, and admits air into pillar, water is extruded into pillar, then eluted with proper amount of methanol, collect wash-out
Liquid, in putting 2ml measuring bottles, and with methanol dilution to scale, shakes up, and obtains final product.
Determination method is accurate respectively to draw the above-mentioned μ l of mixed reference substance solution 5,10 μ l, 15 μ l, 20 μ l, 25 μ l, injects liquid phase
Chromatograph, determines peak area, and with peak area as ordinate, sample size is abscissa, draws standard curve.Another accurate absorption is above-mentioned
The μ l of need testing solution 20~25, inject liquid chromatograph, determine peak area, equivalent to Huang from test sample is read on standard curve
The amount of aspertoxin B1, calculates, and obtains final product.
Result judgement：This product contains AFB per 1000g15 μ g must not be crossed.
Sulfur dioxide residual quantity
Instrument and apparatus：Medicinal herb grinder, assay balance, pharmacopeia sieve, electric jacket
Reagent and test solution：Hydrogen peroxide, methyl red ethanol solution, 0.01mol/L sodium hydroxide titrations liquid, hydrochloric acid solution
(6mol/L) (reagent is pure using analysis, and experimental water is purified water)
Method：Determined according to sulfur dioxide residual quantity determination method (general rule 2331).Get it filled material or medicine materical crude slice fine powder about 10g, accurate
It is weighed, put in two neck round-bottom flasks, add water 300~400ml.Reflux condensing tube switch feedwater is opened, by upper end E mouthfuls of condenser pipe
Place's one rubber wireway of connection is placed in 100ml conical flasks bottom.3% hydrogenperoxide steam generator 50ml is added in conical flask as absorption
Liquid (end of rubber wireway should be below absorbing liquid liquid level).Using preceding, 3 are added to drip methyl red ethanol solution in absorbing liquid
Indicator (2.5mg/ml), and it is titrated to yellow (i.e. terminal with 0.01mol/L sodium hydroxide titration liquid；If it exceeds terminal,
The absorbent solution should then be given up).Nitrogen is opened, flowmeter adjusting gas flow to about 0.2L/min is used；Open separatory funnel C
Piston, hydrochloric acid solution (6mol/L) 10ml is flowed into cucurbit, be immediately heated solution in two neck flasks to boiling, and keep micro-
Boiling；Boiling water in flask stops heating after 1.5 hours.After absorbing liquid lets cool, it is placed on magnetic stirring apparatus and is stirred continuously, uses
Sodium hydroxide titration liquid (0.01mol/L) is titrated, and is not taken off within 20 seconds to the yellow duration, and by the result blank assay of titration
Correction.
Result judgement：This product sulfur dioxide residual quantity must not cross 150mg/kg.
Extract
Instrument and apparatus：Medicinal herb grinder, assay balance, pharmacopeia sieve, thermostat water bath, electric heating constant-temperature blowing drying box
Reagent and test solution：Ethanol (reagent test solution is pure using analysis, and experimental water is purified water)
Determine and result judgement：Determined according to the hot dipping under ethanol soluble extractives determination method (general rule 2201) item, with 75%
Ethanol as solvent
Test sample about 2~4g is taken, it is accurately weighed, in putting the conical flask of 100~250ml, precision plus 75% ethanol 50~
100ml, close plug, weighed weight after standing 1 hour, connects reflux condensing tube, is heated to boiling, and keep micro-boiling 1 hour.Put
After cold, conical flask, close plug, then weighed weight are removed, the weight of less loss are supplied with 75% ethanol, shaken up, filtered with filter is dried,
Precision measures filtrate 25ml, puts and has dried into the evaporating dish of constant weight, after being evaporated in water-bath, in 105 DEG C of dryings 3 hours, puts
Cooled down 30 minutes in drier, rapid accurately weighed weight.Unless otherwise specified, alcohol-soluble is soaked in calculating test sample with dry product
Go out the content (%) of thing.
Result judgement：This product ethanol soluble extractives must not be less than 12.0%.
Assay
Pinoresinol diglucoside
Reagent and test solution：(wherein methyl alcohol is chromatographically pure, and other reagents are pure using analysis, and experiment is used for methyl alcohol, chloroform
Water is purified water)
Reference substance：Pinoresinol diglucoside reference substance
Method：Determined according to high performance liquid chromatography (general rule 0512).
With octadecylsilane chemically bonded silica as filler；With methanol-water (25: 75) as mobile phase；Detection wavelength is
277nm.Number of theoretical plate is calculated by Pinoresinol diglucoside peak and should be not less than 1000.
The preparation of reference substance solution takes Pinoresinol diglucoside reference substance in right amount, accurately weighed, plus methyl alcohol is made every 1ml
Solution containing 0.5mg, obtains final product.
The preparation of need testing solution takes this product about 3g, is cut into fragment, is kneaded into cotton-shaped, takes about 2g, accurately weighed, puts Soxhlet and carries
Take in device, add chloroform appropriate, be heated to reflux 6 hours, discard chloroform liquid, the dregs of a decoction fling to chloroform, then put rope
In family name's extractor, add methyl alcohol appropriate, be heated to reflux 6 hours, extract solution reclaims methyl alcohol to appropriate, is transferred in 10ml measuring bottles,
Plus methyl alcohol is to scale, shake up, filter, take subsequent filtrate, obtain final product.
Determination method is accurate respectively to draw reference substance solution and each 10 μ l of need testing solution, injects liquid chromatograph, determines, i.e.,
.
Result judgement：This product (C containing Pinoresinol diglucoside32H42O16) 0.11% must not be less than.
Microbial limit
Detection of Salmonella takes this product 10g, with the pancreas junket soybean of aseptic inoculation to appropriate volume (tested through method applicability and determined)
In peptone fluid nutrient medium, mix, by non-sterile product limit test of microbe：Control bacteria examination method is checked.
Result judgement：Detection of Salmonella must not be detected (10g).
Bile tolerance gram-negative bacteria takes this product, with aseptic pancreas junket soya peptone fluid nutrient medium as diluent, is made 1: 10
Test liquid, mixes, by non-sterile product limit test of microbe：Control bacteria examination method is checked.
Result judgement：Bile tolerance gram-negative bacteria should be less than 104cfu(1g)。
Claims (3)
1. the quality standard of the bark of eucommia qualitative, quantitative prepared slices of Chinese crude drugs, it is characterised in that：In current edition《Chinese Pharmacopoeia》Quality standard
On the basis of increase medicine bits impurity, heavy metal and harmful element, Residual Levels of Organochlorine Pesticides, AFB1, sulfur dioxide it is residual
Allowance, and the standard limits of the Pinoresinol diglucoside in assay are improved to 0.11% from 0.10%.
2. the quality standard of the bark of eucommia qualitative, quantitative prepared slices of Chinese crude drugs as described in claim 1, it is characterised in that：
Medicine is considered impurity to be worth doing and is determined according to determination of foreign matter method (general rule 2301), should cross 3%.
Heavy metal and harmful element are determined according to lead, cadmium, arsenic, mercury, copper determination method (general rule 2321), and this product is leaded must not to cross 8mg/
Kg, cadmium must not cross 0.8mg/kg, arsenic and must not cross 4mg/kg, mercury and must not cross 0.8mg/kg, copper and must not cross 20mg/kg.
Residual Levels of Organochlorine Pesticides according to persticide residue determination method (method of general rule 0,512 first) determine, this product containing total BHC (α-
BHC, β-BHC, γ-BHC, δ-BHC sums) must not cross 0.2mg/kg, total DDT (pp '-DDE, pp '-DDD, op '-DDT,
Pp '-DDT sums) 0.2mg/kg, pentachloronitrobenzene must not be crossed 0.1mg/kg must not be crossed.
AFB1Determined according to aflatoxin determination method (general rule 2351), this product contains AFB15 μ g/ must not be crossed
kg。
Sulfur dioxide residual quantity is determined according to sulfur dioxide residual quantity determination method (general rule 2331), and this product sulfur dioxide residual quantity must not
Cross 150mg/kg.
3. the manufacturing process of the bark of eucommia qualitative, quantitative prepared slices of Chinese crude drugs, it is characterised in that prepare the bark of eucommia prepared slices of Chinese crude drugs, including following step
Suddenly：
A10, net system：The impurity that is mixed in the bark of eucommia of removing and the product that go mouldy etc., to reach clean or to be processed further treatment.Note
Meaning：The bark of eucommia must not directly contact ground after cleaning.
A20, demulcen：The bark of eucommia after net system is put into Xi Run ponds, water spray heap profit 16-24h, is thoroughly run through to the bark of eucommia.Note：The bark of eucommia
Need to run through, it is soft or hard suitable inside and outside the bark of eucommia.
A30, remove tertia：The bark of eucommia that will be run through removal tertia.
A40, cutting：Broken 0.3~1mm.Operated by fully automatic high-speed slicer operational procedure, mix up knife away from the bark of eucommia is tried
Cut, detected with slide measure, adjust cutting width, formally cut medicine after meeting the requirements again.
A50, drying：It is dried using heated-air circulation oven, the bark of eucommia is laid on baking oven shelf, paving thickness is uniform, thickness
In below 3cm.Switch is opened, heater switch, blower fan is opened, 60 ± 2 DEG C are dried in temperature, and design temperature is reached in temperature
After dry 6-8h, drying is finished, and closes heater switch, continues to dry, and treats that the temperature inside the box is fallen to 35~40 DEG C, closes blower fan.
Post personnel need to fill in intermediate products and please examine list after drying, hand over Quality Mgmt Dept to carry out moisture inspection by QA samplings.
A60, packaging：Packed according to the requirement of this product packing specification.Need to check make-up room before packaging, confirm packaging life
Clearing out a gathering place for producing line has been completed, and checks whether packaging material meet the requirements.Inner packing：Being adjusted in equipment needs printing
Date of manufacture, lot number, QA monitoring, the bark of eucommia for weighing predetermined weight are put into hopper, are sealed with sealing machine, it is desirable to accomplish that sealing is tight
It is close, smooth, attractive in appearance.External packing：Adjusted in equipment the date of manufacture and lot number that need to be printed, QA monitoring, in external packing cases
Upper printing lot number, date of manufacture, should be noted whether lot number and date of manufacture are clear in print procedure.By the drink after the completion of inner packing
Piece and survey report are put into outsourcing box, 4 bags/box.Every 10 box medicine materical crude slice is inserted in 1 heat shrinkage film, carries out thermal contraction；Heat
It is fitted into after contraction in big carton, 240 boxes/case.In operating process, QA is inspected by random samples at any time.Post personnel need to fill in finished product and ask after packaging
Inspection is single, hands over Quality Mgmt Dept to carry out product examination by QA samplings.
A70, finished product：Post personnel need to fill in finished product and please examine list after packaging, hand over Quality Mgmt Dept to carry out product examination by QA samplings.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108261437A (en) * | 2018-01-29 | 2018-07-10 | 江西青春康源中药饮片有限公司 | A kind of concocting method suitable for Cortex Eucommiae cutting |
| CN110887921A (en) * | 2019-11-05 | 2020-03-17 | 广东省测试分析研究所（中国广州分析测试中心） | Method for efficiently and rapidly analyzing characteristic volatile components of eucommia leaves and fermentation product thereof |
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| CN108261437A (en) * | 2018-01-29 | 2018-07-10 | 江西青春康源中药饮片有限公司 | A kind of concocting method suitable for Cortex Eucommiae cutting |
| CN110887921A (en) * | 2019-11-05 | 2020-03-17 | 广东省测试分析研究所（中国广州分析测试中心） | Method for efficiently and rapidly analyzing characteristic volatile components of eucommia leaves and fermentation product thereof |
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