CN106706833A - Quality standard and production process of qualitative and quantitative traditional Chinese medicine decoction pieces containing ginkgo leaves - Google Patents
Quality standard and production process of qualitative and quantitative traditional Chinese medicine decoction pieces containing ginkgo leaves Download PDFInfo
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- CN106706833A CN106706833A CN201610368057.6A CN201610368057A CN106706833A CN 106706833 A CN106706833 A CN 106706833A CN 201610368057 A CN201610368057 A CN 201610368057A CN 106706833 A CN106706833 A CN 106706833A
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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
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
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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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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N2021/3129—Determining multicomponents by multiwavelength light
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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
- G01N2030/025—Gas chromatography
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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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Abstract
The invention provides safe, efficient and convenient traditional Chinese medicine decoction pieces containing ginkgo leaves. A production process of the qualitative and quantitative traditional Chinese medicine decoction pieces containing ginkgo leaves adopts a processing process, the traditional Chinese medicine decoction pieces are prepared from ginkgo leaves conforming to a quality standard, meanwhile, the quality standard of the ginkgo leaf decoction pieces is provided, related detection items of the decoction pieces are formulated on the basis of existing traditional Chinese medicinal material quality standards, standard limits of total flavonol glycosides and terpene lactones in content measurement are increased, the quality of the ginkgo leaf decoction pieces can be effectively controlled, and the quality standard of drugs is icreased, and the medication safety is improved.
Description
Technical field
The present invention relates to the field of Chinese medicines, specially the quality standard of the ginkgo leaf qualitative, quantitative prepared slices of Chinese crude drugs, operational procedure with
Manufacturing process.
Background technology
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.
This product is the dried leaf of Ginkgoaceae plant Ginkgo biloba Ginkgo biloba L..Ginkgo leaf has as conventional Chinese medicine
Powerful potentiality to be exploited.Ginkgo leaf rich in flavonoids, terpene, ginnol, shikimic acid, sitosterol, alkaloid, PI,
The active ingredients such as several amino acids, mineral matter, polysaccharide, OPC, tannin, ginkgolic acid, wax, chlorophyll, its function and master
Control as promoting blood circulation and removing blood stasis, remove obstruction in channels to relieve pain, astringe the lung and relieving asthma, change turbid lipid-loweringing.For obstruction of collaterals by blood stasis, chest impediment and cardialgia, hemiplegia, the deficiency syndrome of the lung is coughed
Breathe heavily, hyperlipidemia.Traditional decoction takes more time and effort consuming, therefore brews the ginkgo leaf Chinese medicine taken drink in the urgent need to a kind of
Piece.
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).Ginkgo leaf because
Environmental pollution and the quality problems such as heavy metals exceeding standard (Zhang Xuemei Chengdu atmosphere heavy metal pollution ginkgo leaf study on monitoring【D】.
Chengdu：Chengdu University of Technology, 2014).
Problem to be solved by this invention is to solve the exceeded quality problems of Chinese medicine residues of pesticides, the residues of pesticides of Chinese medicine
Mainly there are 3 aspects in source：One is sprayed to control disease, worm, crop smothering or coordinate plant growth in the growth course of Chinese medicine
The agricultural chemicals applied.Two is pollution of the Chinese medicine planting environment Pesticides to medicinal material.Such as soil, water source, air around medicinal material growth
Pesticides etc., are entered in medicinal plant body by absorbed organs such as root, leaves.Three be medicinal material in processing, storage in order to protect
Card quality and other articles that the agricultural chemicals or medicinal material that spray are contacted and the agricultural chemicals be infected with.Such as some medicinal material producing regions, agriculture is being applied
Soon harvesting is begun to after medicine；Contain residues of pesticides higher in the auxiliary material added during medicinal material processing；Using packing, transported
(the Chinese medicine residues of pesticides present Research such as pretty high such as Chinese medicine is packed, transported to the medium of agricultural chemicals【J】Medicinal plant cigarette
Grass, 2008).
Brief description of the drawings
Accompanying drawing 1 is ginkgo leaf 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 ginkgo leaf qualitative, quantitative prepared slices of Chinese crude drugs that the present invention is provided
Skill, in current edition《Chinese Pharmacopoeia》Coherent detection standard is worked out on the basis of the ginkgo leaf Chinese medicine standard of quality standard, and is increased
Dosing bits impurity, heavy metal and harmful element, Residual Levels of Organochlorine Pesticides, AFB1, sulfur dioxide residual quantity, and will
The standard limits of the total flavonoids in assay are improved to 0.44%, terpene lactone (ginkalide A, ginkgo from 0.40%
The total amount of lactone B, ginkalide C and Bilobalide) standard limits are improved to 0.28% from 0.25%, and by specific operation
Produce the ginkgo leaf prepared slices of Chinese crude drugs of fragment 0.4mm, it is ensured that the prepared slices of Chinese crude drugs meet high standard quality requirements.
The manufacturing process of the ginkgo leaf 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 ginkgo leaf of removing and the product that go mouldy etc., to reach clean or to be processed further place
Reason.Note：Ginkgo leaf must not directly contact ground after cleaning.
A20, cleaning：Ginkgo leaf is placed in wash pond after net system, is cleaned up to without silt, quickly to be robbed during cleaning
Wash, reduce ginkgo leaf soak time in water.Heap profit 2-3h, thoroughly runs through to ginkgo leaf after the completion of cleaning.
A30, cutting：Operated by fully automatic high-speed slicer operational procedure, mix up knife away from 0.4mm, carry out cutting medicine.
A40, drying：It is dried using heated-air circulation oven, ginkgo leaf is laid on baking oven shelf, paving thickness is equal
Even, thickness is in below 3cm.Switch is opened, heater switch, blower fan is opened, 60 ± 2 DEG C are dried in temperature, are reached in temperature
5-7h is dried after design 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, closed
Close 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.
A50, 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 ginkgo leaf for weighing predetermined weight are put into hopper, are sealed with sealing machine, it is desirable to accomplish
Sealing 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 outsourcing
Lot number, date of manufacture are printed on mounted box, should be noted whether lot number and date of manufacture are clear in print procedure.Inner packing is completed
Medicine materical crude slice and survey report afterwards is 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.
A60, 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.
In current edition《Chinese Pharmacopoeia》Coherent detection standard is worked out on the basis of the ginkgo leaf Chinese medicine standard of quality standard,
And increase medicine bits impurity, heavy metal and harmful element, Residual Levels of Organochlorine Pesticides, AFB1, sulfur dioxide residual quantity,
And by the standard limits of the total flavonoids in assay from 0.40% improve to 0.44%, terpene lactone (ginkalide A,
The total amount of ginkolide B, ginkalide C and Bilobalide) standard limits are improved to 0.28% from 0.25%.The ginkgo leaf of revision
The quality standard of the qualitative, quantitative prepared slices of Chinese crude drugs is as follows：
Ginkgo leaf medicine materical crude slice
Phonetic title：Yinxingye Yinpian
Packaging：Fine aluminium composite film packaging.
【Proterties】Take this product appropriate, observe in the sunlight, this product is irregular broken, and body is light, smells it, and gas is micro-, tastes it, and taste is micro-
It is bitter.
Differentiate
Thin layer differentiates
Instrument and apparatus：Medicinal herb grinder, assay balance, pharmacopeia sieve, supersonic wave cleaning machine, thermostat water bath, sample applicator,
Expansion cylinder, lamellae, three use ultraviolet device
Reagent and test solution：Ethanol, 4% SAS, 3% alchlor ethanol solution, ethyl acetate, butanone, formic acid,
Acetone, toluene, methyl alcohol, aceticanhydride
Determine and result judgement
This product powder 1g, plus 40% ethanol 10ml are taken, is heated to reflux 10 minutes, let cool, filtered, take filtrate as test sample
Solution.Ginkgo leaf control medicinal material 1g separately is taken, control medicinal material solution is made in the same way of.According to thin-layered chromatography (general rule 0502) experiment, inhale
Each 6 μ l of above two solution are taken, is put respectively on the same silica gel g thin-layer plate prepared with 4% SAS, with acetic acid second
Ester-butanone-formic acid-water (5: 3: 1: 1) is solvent, is launched, and is taken out, and is dried, and is sprayed with 3% alchlor ethanol solution, hot blast
Drying, puts and inspect under ultraviolet lamp (365nm).
Result judgement：In test sample chromatogram, on position corresponding with control medicinal material chromatogram, show the fluorescence master of same color
Spot.
This product powder 1g, plus 50% acetone soln 40ml are taken, is heated to reflux 3 hours, filtered, filtrate is evaporated, and residue adds water
20ml makes dissolving, is shaken with ethyl acetate and extracted 2 times, and each 20ml, combined ethyl acetate liquid is evaporated, and residue adds 15% ethanol
5ml makes dissolving, adds on processed good polyamide column (30~60 mesh, 1g, internal diameter is 1cm, uses water wet method dress post), with 5%
Ethanol 40ml is eluted, and collects eluent, puts and ethanol is boiled off in water-bath, and aqueous are shaken with ethyl acetate and extracted 2 times, each 20ml,
Combined ethyl acetate liquid, is evaporated, and residue adds the acetone 1ml to make dissolving, used as need testing solution.Separately take ginkalide A reference substance, silver
Apricot lactone B reference substances, ginkalide C reference substance and Bilobalide reference substance, plus acetone are made each bilobalide-containing A of every 1ml
0.5mg, ginkolide B 0.5mg, ginkalide C 0.5mg, the mixed solution of Bilobalide 1mg, as reference substance solution.According to
Thin-layered chromatography (general rule 0502) is tested, and draws each 5ul of above two solution, is put respectively in same with 4% SAS system
On standby silica gel g thin-layer plate, with toluene-ethyl acetate-acetone-methanol (10: 5: 5: 0.6) as solvent, opened up below 15 DEG C
Open, take out, dry, smoked 15 minutes in aceticanhydride steam, heated 30 minutes in 140~160 DEG C, put ultraviolet lamp (365nm)
Under inspect.
Result judgement：In test sample chromatogram, on position corresponding with reference substance chromatogram, show the fluorescent spot of same color
Point.
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, medication is sifted out medicine bits, merged, weigh, counts
Calculate its amount (%) in test sample.
Result judgement：This product impurity must not cross 2%.
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 12.0%.
Total ash
Instrument and apparatus：Medicinal herb grinder, assay balance, pharmacopeia sieve, Muffle furnace, electric furnace, crucible
Determine and result judgement：Determined according to Ash determination method (general rule 2302).
2~3g of test sample (as acid-insoluble ash must be determined, can use 3~5g of test sample) is taken, the earthenware of ignition to constant weight is put
In crucible, weighed weight (accurately to 0.01g) is slowly red-hot, notes avoiding burning, when carbonizing completely, gradually rises temperature extremely
500~600 DEG C, make ashing completely and to constant weight.According to residue weight, the content (%) of total ash in test sample is calculated.
Result judgement：This product total ash must not cross 10.0%.
Acid-insoluble ash
Instrument and apparatus：Medicinal herb grinder, assay balance, pharmacopeia sieve, Muffle furnace, electric furnace, crucible
Reagent and test solution：Watery hydrochloric acid, purified water
Determine and result judgement：Determined according to Ash determination method (general rule 2302).
The ash content obtained by item is taken, watery hydrochloric acid about 10ml is carefully added into crucible, crucible is covered with surface plate, put water-bath
Upper heating 10 minutes, surface plate is rinsed with hot water 5ml, and washing lotion is incorporated in crucible, is filtered with ashless filter paper, and the residue in crucible is used
Wash on filter paper, and wash to washing lotion and do not show chloride reacts.Filter residue is dried together with the same crucible of filter paper dislocation,
Ignition to constant weight.According to residue weight, the content (%) of acid-insoluble ash in test sample is calculated.
Result judgement：This product acid-insoluble ash must not cross 2.0%.
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 hydroxyl is added dropwise
Amine aqueous 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, be slowly heated in 120 DEG C reddish brown
Color 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
It is even, 5% hydroxylamine hydrochloride solution to aubergine is added dropwise and just disappears, it is transferred in 10ml measuring bottles, wash container, the washing lotion amount of being incorporated in water
In bottle, and scale is diluted to, shaken up, be centrifuged if necessary, take supernatant, obtained 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, pp '-DDE, pp '-DDD, op '-DDT, pp '-DDT, PCNB
Agricultural chemical reference substance
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) (pp '-DDE, pp '-DDD, op '-DDT, pp '-DDT) and pentachloronitrobenzene (PCNB) appropriate agricultural chemical reference substance, use
Petroleum ether (60~90 DEG C) is respectively prepared solution of every 1ml containing about 4~5 μ g, obtains 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,
Must not cross 0.2mg/kg, pentachloronitrobenzene must not mistake for total DDT (pp '-DDE, pp '-DDD, op '-DDT, pp '-DDT sums)
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, adds chlorine
Change sodium 3g, precision adds 70% methanol solution 75ml, 2 minutes (mixing speed is more than 11000 revs/min) of high-speed stirred, centrifugation 5
Minute (2500 revs/min of centrifugal speed), precision measures supernatant 15ml, puts in 50ml measuring bottles, is diluted with water to scale, shakes
It is even, with (0.45 μm) filtration of miillpore filter, subsequent filtrate 20.0ml is measured, by immune affinity column, flow velocity 3ml per minute uses water
20ml is eluted, and eluent is discarded, and admits air into pillar, and water is extruded into pillar, then is eluted with proper amount of methanol, collects eluent,
In putting 2ml measuring bottles, and with methanol dilution to scale, shake up, obtain 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, then
The absorbent solution should be given up).Nitrogen is opened, flowmeter adjusting gas flow to about 0.2L/min is used；Open separatory funnel C's
Piston, makes hydrochloric acid solution (6mol/L) 10ml flow into cucurbit, is immediately heated the 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 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, use dilute second
Alcohol makees solvent
Test sample about 2~4g is taken, it is accurately weighed, in putting the conical flask of 100~250ml, precision plus 50~100ml of ethanol,
Close plug, weighed weight after standing 1 hour, connects reflux condensing tube, is heated to boiling, and keep micro-boiling 1 hour.After letting cool, take
Inferior pyramidal bottle, close plug, then weighed weight, the weight of less loss is supplied with ethanol, is shaken up, and is filtered with filter is dried, and precision measures filter
Liquid 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 cold in drier
But 30 minutes, rapid accurately weighed weight.Unless otherwise specified, the content of ethanol soluble extractives in test sample is calculated with dry product
(%).
Result judgement：This product ethanol soluble extractives must not be less than 25.0%.
Assay
Total flavonoids
Instrument and apparatus：Medicinal herb grinder, assay balance, pharmacopeia sieve, thermostat water bath, liquid chromatograph
Reagent and test solution：Methyl alcohol, chloroform, hydrochloric acid, petroleum ether (30-60 DEG C), phosphoric acid, tetrahydrofuran, purified water (its
Middle methyl alcohol is chromatographically pure, and other reagents are pure using analysis, and experimental water is purified water)
Reference substance：Quercetin reference substance, Kaempferide reference substance, Isorhamnetin reference substance, ginkalide A reference substance, ginkgo
Lactone B reference substances, ginkalide C reference substance, Bilobalide reference substance
Method：Determined according to high performance liquid chromatography (general rule 0512).
Chromatographic condition is with system suitability with octadecylsilane chemically bonded silica as filler；With the phosphorus of methyl alcohol -0.4%
Acid solution (50: 50) is mobile phase；Detection wavelength is 360nm.Number of theoretical plate is calculated by Quercetin peak and should be not less than 2500.
The preparation of reference substance solution takes Quercetin reference substance, Kaempferide reference substance, Isorhamnetin reference substance in right amount, and precision claims
Determine, plus methyl alcohol is made every 1ml containing the μ g of Quercetin 30, the μ g of Kaempferide 30, the mixed solution of the μ g of Isorhamnetin 20, obtains final product.
The preparation of need testing solution takes powder about 1g in this product, accurately weighed, in putting apparatus,Soxhlet's, plus chloroform backflow
Extract 2 hours, discard chloroform liquid, the dregs of a decoction are volatilized, plus methanol eddy extract 4 hours, extract solution is evaporated, residue add methyl alcohol-
25% hydrochloric acid solution (4: 1) mixed solution 25ml, is heated to reflux 30 minutes, lets cool, and is transferred in 50ml measuring bottles, and adds methyl alcohol extremely
Scale, shakes up, and obtains 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,
The content of Quercetin, Kaempferide and Isorhamnetin is calculated respectively, and the content of total flavonoids is converted into as the following formula.
Total flavonoids content=(quercetin content+Kaempferia galanga cellulose content+Isorhamnetin content) × 2.51
Result judgement：This product is calculated by dry product, and 0.44% must not be less than containing total flavonoids.
Terpene lactone
Chromatographic condition is with system suitability with octadecylsilane chemically bonded silica as filler；With methyl alcohol-tetrahydrochysene furan
Mutter-water (25: 10: 65) is mobile phase；EISD is detected.Number of theoretical plate is calculated by Bilobalide peak and should be not less than
3000。
The preparation of reference substance solution takes ginkalide A reference substance, ginkolide B reference substance, ginkalide C reference substance, white
Fruit lactone reference substance is appropriate, accurately weighed, plus 50% methyl alcohol is made every 1ml bilobalide-containings A 0.18mg, ginkolide B
0.08mg, ginkalide C 0.10mg, the mixed solution of Bilobalide 0.20mg, obtain final product.
The preparation of need testing solution takes powder about 1.5g in this product, accurately weighed, in putting apparatus,Soxhlet's, plus petroleum ether (30
~60 DEG C) refluxing extraction 1 hour in 70 DEG C of water-baths, petroleum ether (30~60 DEG C) liquid is discarded, the dregs of a decoction and filtration paper cylinder wave most oil
Ether, is placed in 60 DEG C of baking ovens and dries, then adds methanol eddy to extract 6 hours, and extract solution is evaporated, and residue adds the methyl alcohol to make dissolving, shifts
Into 10ml measuring bottles, ultrasonically treated (power 300W, frequency 50kHZ) 30 minutes takes out, lets cool, plus methyl alcohol is to scale, shakes up,
Stand, precision measures supernatant 5ml, (200~300 mesh, 3g, internal diameter is 1cm, is filled with methanol wet to add acidic alumina column
Post) on, eluted with methyl alcohol 25ml, eluent is collected, to doing, residue methyl alcohol 5m1 is transferred to 10ml measuring bottles to recycling design by several times
In, add water about 4.5ml, ultrasonically treated (power 300W, frequency 50kHz) 30 minutes, takes out, and lets cool, plus methyl alcohol is to scale, shakes
It is even, obtain final product.
Determination method is accurate respectively to draw the μ l of reference substance solution 10,20 μ l, the μ l of need testing solution 10~20, injects liquid chromatogram
Instrument, is determined, and ginkalide A, ginkolide B, ginkalide C and Bilobalide are calculated respectively with external standard two-point method logarithmic equation
Content, obtains final product.
Result judgement：This product is calculated by dry product, containing terpene lactone with ginkalide A (C20H24O9), ginkolide B
(C20H24O10), ginkalide C (C20H24O11) and Bilobalide (C15H18O8) total amount meter, must not be less than 0.28%.
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 ginkgo leaf qualitative, quantitative prepared slices of Chinese crude drugs, it is characterised in that：In current edition《Chinese Pharmacopoeia》Quality standard
Ginkgo leaf Chinese medicine standard on the basis of work out coherent detection standard, and increase medicine bits impurity, heavy metal and harmful element, have
Machine chloro pesticide residual quantity, AFB1, sulfur dioxide residual quantity, and the standard of the total flavonoids in assay is limited
Spend from 0.40% improve to 0.44%, terpene lactone (ginkalide A, ginkolide B, ginkalide C and Bilobalide it is total
Amount) standard limits are improved to 0.28% from 0.25%.
2. the quality standard of the ginkgo leaf 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 2%.
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 ginkgo leaf qualitative, quantitative prepared slices of Chinese crude drugs, it is characterised in that prepare the ginkgo leaf Chinese medicine of fragment 0.4mm
Medicine materical crude slice, comprises the following steps：
A10, net system：The impurity that is mixed in ginkgo leaf of removing and the product that go mouldy etc., to reach clean or to be processed further treatment.Note
Meaning：Ginkgo leaf must not directly contact ground after cleaning.
A20, cleaning：Ginkgo leaf is placed in wash pond after net system, is cleaned up to quickly being robbed without silt, during cleaning and is washed, and is subtracted
Few ginkgo leaf soak time in water.Heap profit 2-3h, thoroughly runs through to ginkgo leaf after the completion of cleaning.
A30, cutting：Operated by fully automatic high-speed slicer operational procedure, mix up knife away from 0.4mm, carry out cutting medicine.
A40, drying：It is dried using heated-air circulation oven, ginkgo leaf is laid on baking oven shelf, paving thickness is uniform, it is thick
Degree is in below 3cm.Switch is opened, heater switch, blower fan is opened, 60 ± 2 DEG C are dried in temperature, setting temperature is reached in temperature
5-7h is dried after degree, 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.
A50, 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 ginkgo leaf for weighing predetermined weight are put into hopper, are sealed with sealing machine, it is desirable to accomplish sealing
Tightly, it is 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 box
Lot number, date of manufacture are printed on son, 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 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；
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 finished product after packaging
List please be examine, hands over Quality Mgmt Dept to carry out product examination by QA samplings.
A60, 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 (1)
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