CN106771012A - The quality standard and manufacturing process of the motherwort qualitative, quantitative prepared slices of Chinese crude drugs - Google Patents
The quality standard and manufacturing process of the motherwort qualitative, quantitative prepared slices of Chinese crude drugs Download PDFInfo
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- CN106771012A CN106771012A CN201610368132.9A CN201610368132A CN106771012A CN 106771012 A CN106771012 A CN 106771012A CN 201610368132 A CN201610368132 A CN 201610368132A CN 106771012 A CN106771012 A CN 106771012A
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- Prior art keywords
- motherwort
- solution
- product
- standard
- crude drugs
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- ALABRVAAKCSLSC-UHFFFAOYSA-N rutin Natural products CC1OC(OCC2OC(O)C(O)C(O)C2O)C(O)C(O)C1OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5 ALABRVAAKCSLSC-UHFFFAOYSA-N 0.000 description 1
- 235000005493 rutin Nutrition 0.000 description 1
- 229960004555 rutoside Drugs 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 238000003900 soil pollution Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 206010042772 syncope Diseases 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/15—Medicinal preparations ; Physical properties thereof, e.g. dissolubility
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/30—Staining; Impregnating ; Fixation; Dehydration; Multistep processes for preparing samples of tissue, cell or nucleic acid material and the like for analysis
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- 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
-
- 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
-
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
- G01N5/045—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder for determining moisture content
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2873—Cutting or cleaving
-
- 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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
Abstract
The invention provides one kind is safe efficient, the easily motherwort prepared slices of Chinese crude drugs.The motherwort qualitative, quantitative prepared slices of Chinese crude drugs manufacturing process that the present invention is provided, using a kind of processing procedure, the motherwort that quality standard will be met is prepared into the suitable prepared slices of Chinese crude drugs, can brew and take change traditional decoction instructions of taking, there is provided a kind of motherwort prepared slice quality standard simultaneously, increase coherent detection project on the basis of existing quality standard, and improve the stachydrine hydrochloride in assay, the standard limits of hydrochloric acid leonurine, quality that can be effectively to motherwort medicine materical crude slice is controlled, the quality standard of medicine is improve, drug safety is increased.
Description
Technical field
The present invention relates to the field of Chinese medicines, specially the quality standard of the motherwort qualitative, quantitative prepared slices of Chinese crude drugs, operational procedure with
Manufacturing process.
Background technology
Motherwort (scientific name:Leonuri herba), also known as motherwort, female grass, benefit mother Chinese mugwort, triangle linseed, four stupefied sons, it is
The fresh or dry aerial parts of labiate motherwort.History is carried《Sheng Nong's herbal classic》Top grade is classified as, motherwort contains motherwort
Alkali, stachydrine, rutin sophorin, fumaric acid, different motherwort element, motherwort qin element etc., with promoting blood circulation, menstruation regulating, disappear water effect, is used for
Irregular menstruation, threatened abortion difficult labour, placenta retension, postpartum anemic fainting, abdominal pain due to blood stasis, metrorrhagia and metrostaxis etc., are good medicine for women,
Informal dress can channel warming and blood nourishing, stasis-dispelling and pain-killing.With the development of modern pharmacological research, except meeting being got interested to womb for traditional cognitive
The effect of putting forth energy is outer, and motherwort can reduce coronary resistance, reducing heart rate etc. to Cardiovascular, also strengthen the work(of immunity of organisms
Effect, with powerful potentiality to be exploited.
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 motherwort medicine materical crude slice curative effect for solving in the market is not obvious, and motherwort body
The content of interior heavy metal element and degree Cheng Zhengguan (the Jinhua suburbs motherwort such as Chen Jianhua and the soil of The Heavy Metal Contaminated Soil
The analysis of 4 heavy metal species contents in earth【J】Zhejiang Normal University's journal, 2004), the problems such as increasingly serious soil pollution, benefit
The monitoring of Brittle Falsepimpernel Herb heavy-metal residual, Monitoring Pesticide Residues are shouldered heavy responsibilities, and send out imperative.
Brief description of the drawings
Accompanying drawing 1 is motherwort 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 motherwort qualitative, quantitative prepared slices of Chinese crude drugs of this bright offer
Skill, increases medicine bits impurity, heavy metal and harmful element, Residual Levels of Organochlorine Pesticides, AFB1, sulfur dioxide residue
Amount, assay, and the standard limits of the stachydrine hydrochloride in assay are carried from 0.40% (motherwort Chinese medicine standard)
Up to 0.44%, the standard limits of hydrochloric acid leonurine are improved to 0.044% from 0.040% (motherwort Chinese medicine standard).And
The motherwort prepared slices of Chinese crude drugs of 0.3~1mm of slice thickness are produced by specific operation, it is ensured that the prepared slices of Chinese crude drugs meet high standard high-quality
Requirement.
The manufacturing process of the Herba Saussureae Involueratae 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 motherwort of removing and the product that go mouldy etc., to reach clean or to be processed further place
Reason.
A20, demulcen:Motherwort after net system is put into Xi Run ponds, water spray heap profit 16-24h, is thoroughly run through to motherwort.
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, motherwort 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
6-8h 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 medicinal material 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.
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.
Increase medicine bits impurity, heavy metal and harmful element, Residual Levels of Organochlorine Pesticides, AFB1, sulfur dioxide
Residual quantity, assay, and by the standard limits of the stachydrine hydrochloride in assay from 0.40% (motherwort Chinese medicine mark
It is accurate) improve to 0.44%, the standard limits of hydrochloric acid leonurine are improved extremely from 0.040% (motherwort Chinese medicine standard)
0.044%.The quality standard of the revised motherwort qualitative, quantitative prepared slices of Chinese crude drugs is as follows:
Motherwort medicine materical crude slice
Phonetic title:Yimucao Yinpian
Packaging:Fine aluminium composite film packaging.
【Proterties】Take this product appropriate, observe in the sunlight, this product is in irregular section.It is smelt, gas is micro-, taste it, mildly bitter flavor.
Sweet, pungent, slight 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, electric heating constant-temperature blowing drying box, three use ultraviolet device
Reagent and test solution:Absolute ethyl alcohol, acetone, hydrochloric acid, dilute bismuth potassium iodide test solution, (reagent is used ferric trichloride test solution
Analysis is pure, and experimental water is purified water)
Control medicinal material and reference substance:Stachydrine hydrochloride reference substance
Take stachydrine hydrochloride【Assay】Need testing solution 10ml under, is evaporated, and it is molten that residue adds absolute ethyl alcohol 1ml to make
Solution, centrifugation, takes supernatant as need testing solution.Stachydrine hydrochloride reference substance is separately taken, plus absolute ethyl alcohol is made every 1ml containing 1mg
Solution, as reference substance solution.According to thin-layered chromatography (general rule 0502) experiment, each 5~10ul of above two solution is drawn, point
Other point, with acetone-absolute ethyl alcohol-hydrochloric acid (10: 6: 1) as solvent, launches on same silica gel g thin-layer plate, takes out, and dries,
Heated 15 minutes at 105 DEG C, let cool, spray is aobvious to spot with dilute bismuth potassium iodide test solution-ferric trichloride test solution (10: 1) mixed solution
Color is clear.Result judgement:In test sample chromatogram, on position corresponding with reference substance chromatogram, show the spot of same color.
Result judgement:In test sample chromatogram, on position corresponding with reference substance chromatogram, show the spot of same color.
Check
Medicine bits, impurity
Instrument and apparatus:Medicinal herb grinder, assay balance, pharmacopeia sieve
Determine and result judgement:Determined according to determination of foreign matter method (general rule 2301).
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).Test sample is taken (to be approximately equivalent in right amount
1~4ml of water content), it is accurately weighed, in putting the short-neck round bottom flask of 500ml, plus toluene about 200ml, add if necessary dry,
Clean to connect instrument without the small ceramics of glaze several pieces or bead number, autocondensation pipe top adds toluene to being full of determination of moisture
The narrow thin portion of pipe point.Round-bottomed flask is put in electric jacket or is slowly heated with other proper methods, when toluene comes to life, adjust
Section temperature, makes per second to distillate 2 drops.Treat that moisture is distillated completely, that is, when the water for determining pipe scale part is not further added by, by condenser pipe
It is internal first to use toluene rinse, then brushed or other proper methods with the full length for dipping in toluene, the toluene that will adhere on tube wall is pushed, and is continued
Distillation 5 minutes, is let cool to room temperature, and provision for disengagement is attached on the tube wall of determination of moisture pipe if any water, can use the copper wire for dipping in toluene
Push, placement makes moisture be kept completely separate (methylenum careuleum powder can be added a small amount of, water is dyed blueness, to separate observation) with toluene.
Water is reviewed, and is calculated as the water content (%) of test sample.Result judgement:This product moisture must not cross 13.0%.
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 is taken (as acid must be determined not
Dissolubility ash content, can use 3~5g of test sample), to put in the crucible of ignition to constant weight, weighed weight (accurately to 0.01g) is slowly vehement
Heat, notes avoiding burning, when carbonizing completely, gradually rises temperature to 500~600 DEG C, makes ashing completely and to constant weight.According to
Residue weight, calculates the content (%) of total ash in test sample.Result judgement:This product total ash must not cross 11.0%.
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, system
Into the solution of the μ g of every 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 points is made of 2% salpeter solution
The solution of not leaded 0ng, 5ng, 20ng, 40ng, 60ng, 80ng.Precision measures 1ml respectively, and precision adds and contains 1% ammonium dihydrogen phosphate
With the solution 0.5ml of 0.2% magnesium nitrate, mix, precision draws 20 μ l injection graphite furnace atomizers, mensuration absorbance, to inhale
Luminosity is ordinate, 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, system
Into solution of every 1ml containing the μ g of cadmium (Cd) 1, obtain 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 often
The solution of 1ml 0ng containing cadmium, 0.8ng, 2.0ng, 4.0ng, 6.0ng, 8.0ng respectively.It is accurate respectively to draw 10 μ l, inject graphite
Stove atomizer, 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, the preparation lower section of sighting target directrix curve
Method mensuration absorbance (if test sample has interference, precision standard liquid, blank solution and each 1ml of need testing solution can be measured respectively,
Precision plus the solution 0.5ml containing 1% ammonium dihydrogen phosphate and 0.2% magnesium nitrate, mix, and determine in accordance with the law), read from standard curve
The content of cadmium (Cd) in need testing solution, calculates, and obtains final product.
The measure (hydride method) of arsenic
Condition determination uses suitable hydride generation system, (faces with containing sodium borohydride and 0.3% sodium hydroxide solution
Use 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, system
Into solution of every 1ml containing the μ g of arsenic (As) 1, obtain 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 often
The solution of 1ml 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 suitable
Amount, sucks hydride generation system, determines absorption value, and with peak area (or absorbance) as ordinate, concentration is abscissa, draws
Standard 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 containing 0.5% sodium borohydride and 0.1% NaOH
Solution (prepared before use) is carrier fluid as reducing agent, hydrochloric acid solution (1 → 100), 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, system
Into the solution of the μ g of every 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, 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 blank solution with need testing solution in right amount, and the method under sighting target directrix curve preparation is determined
The content of mercury (Hg) from need testing solution is read on standard curve, calculates, and obtains 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, system
Into the solution of every μ g of 1ml cuprics (Cu) 10, obtain 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 points is made of 2% salpeter solution
The μ g of other cupric 0,0.05 μ g, 0.2 μ g, 0.4 μ g, 0.6 μ g, the solution of 0.8 μ g.Flame, mensuration absorbance, with extinction are sprayed into successively
It is ordinate to spend, and 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)
Methyl polysiloxane is the fused-silica capillary column (30m × 0.32mm × 0.25 μm) of fixer, the capture of 63Ni-ECD electronics
Detector.230 DEG C of injector temperature, 300 DEG C of detector temperature, Splitless injecting samples.Temperature programming:Initial 100 DEG C, per minute 10
220 DEG C DEG C are risen to, 8 DEG C per minute rise to 250 DEG C, are kept for 10 minutes.Number of theoretical plate calculates 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, puts 10ml measuring bottles
In, scale is diluted to petroleum ether (60~90 DEG C), shake up, obtain final product.
The preparation precision of mixed reference substance solution measures above-mentioned mixing reference substance stock solution, with petroleum ether (60~90 DEG C)
Every 1L is made respectively containing 0 μ g, 1 μ g, 5 μ g, 10 μ g, 50 μ g, 100 μ g, the solution of 250 μ g, is obtained 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
In 100ml conical flask with cover, added water 20ml soaked overnights, and precision adds acetone 40ml, and weighed weight ultrasonically treated 30 minutes, is put
It is cold, then weighed weight, the weight of less loss is supplied with acetone, then add sodium chloride about 6g, precision adds methylene chloride 30ml, weighed heavy
Amount, ultrasound 15 minutes, then weighed weight, the weight of less loss is supplied with dichloromethane, is stood (making layering), and organic phase is moved rapidly
Enter in the 100ml conical flask with cover equipped with appropriate anhydrous sodium sulfate, place 4 hours.Precision measures 35ml, subtracts in 40 DEG C of water-baths
Pressure is concentrated near dry, plus a small amount of petroleum ether (60~90 DEG C) operates cleared to dichloromethane and acetone repeatedly as preceding, uses petroleum ether
(60~90 DEG C) dissolve and are transferred in 10ml tool plug graduated centrifuge tubes, plus petroleum ether (60~90 DEG C) precision is diluted to 5ml, small
The heart adds sulfuric acid 1ml, shakes 1 minute, centrifugation (3000 revs/min) 10 minutes, and precision measures supernatant 2ml, puts tool scale
In concentrate bottle, 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。
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, accurately weighed, puts in two neck round-bottom flasks, and add water 300~400ml.Open back
Stream condenser pipe switch feedwater, 100ml conical flasks bottom is placed in by a rubber wireway is connected at upper end E mouthfuls of condenser pipe.Taper
3% hydrogenperoxide steam generator 50ml is added in bottle as absorbing liquid (end of rubber wireway should be below absorbing liquid liquid level).Make
With preceding, 3 are added to drip methyl red ethanol solution indicator (2.5mg/ml) in absorbing liquid, and dripped with 0.01mol/L NaOH
Determine liquid and be titrated to yellow (i.e. terminal;If it exceeds terminal, then should give up the absorbent solution).Nitrogen is opened, is adjusted using flowmeter
Throttle body flow is to about 0.2L/min;The piston of separatory funnel C is opened, hydrochloric acid solution (6mol/L) 10ml is flowed into cucurbit,
The solution in two neck flasks is immediately heated to boiling, and keeps micro-boiling;Boiling water in flask stops heating after 1.5 hours.Absorb
After liquid lets cool, it is placed on magnetic stirring apparatus and is stirred continuously, titrated with sodium hydroxide titration liquid (0.01mol/L), continues to yellow
20 seconds time was not taken off, and the result of titration is corrected with blank assay.
Result judgement:This product sulfur dioxide residual quantity must not cross 150mg/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) be 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 lambdaex=360nm (or 365nm), emission wavelength lambdaex=450nm.Two phases
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.In another accurate absorption
State the μ l of need testing solution 20~25, inject liquid chromatograph, determine peak area, from test sample is read on standard curve equivalent to
AFB1Amount, calculate, obtain final product.
Result judgement:This product contains AFB per 1000g15 μ g must not be crossed.
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:70% ethanol (reagent is pure using analysis, and experimental water is purified water)
Method:Determined according to the hot dipping under ethanol soluble extractives determination method (general rule 2201) item, use 70% ethanol as solvent.
Test sample about 2~4g is taken, it is accurately weighed, in putting the conical flask of 100~250ml, precision plus 70% 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 70% 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
Stachydrine hydrochloride
Instrument and apparatus:Medicinal herb grinder, assay balance, pharmacopeia sieve, supersonic wave cleaning machine, high performance liquid chromatograph
Reagent and test solution:(wherein acetonitrile is chromatographically pure, and other reagents are pure for analysis, real for acetonitrile, glacial acetic acid, absolute ethyl alcohol
It is purified water to test with water)
Reference substance:Stachydrine hydrochloride reference substance
Method:Determined according to high performance liquid chromatography (general rule 0512).Chromatographic condition is with system suitability with propyl group acyl
Amine bonded silica gel is filler;With the glacial acetic acid solution of acetonitrile -0.2% (80: 20) as mobile phase;Examined with EISD
Survey.Number of theoretical plate presses the calculating of stachydrine hydrochloride peak should not be low by 6000.
The preparation of the preparation reference substance solution of reference substance solution takes stachydrine hydrochloride reference substance in right amount, accurately weighed, plus
70% ethanol is made solution of every 1ml containing 0.5mg, obtains final product.
The preparation for preparing need testing solution of need testing solution takes this product powder (crossing No. three sieves) about 1g, accurately weighed, puts
In conical flask with cover, precision adds 70% ethanol 25ml, and weighed weight is heated to reflux 2 hours, lets cool, then weighed weight, uses
70% ethanol supplies the weight of less loss, shakes up, filtration, takes subsequent filtrate, obtains final product.
Determination method is accurate respectively to draw reference substance solution 5ul, 10ul, and 10~20ul of need testing solution injects liquid chromatogram
Instrument, determines, and is calculated with external standard two-point method logarithmic equation, obtains final product.
Result judgement:This product is calculated by dry product, hydrochloric stachydrine (C7H13NO2HCl 0.44% must not) be less than.
Hydrochloric acid leonurine
Instrument and apparatus:Medicinal herb grinder, assay balance, pharmacopeia sieve, supersonic wave cleaning machine, high performance liquid chromatograph
Reagent and test solution:(wherein acetonitrile is chromatographically pure, and other reagents are pure for analysis, real for acetonitrile, perfluorooctane sulfonate, phosphoric acid
It is purified water to test with water)
Reference substance:Hydrochloric acid leonurine 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 acetonitrile -0.4%
0.1% phosphoric acid solution (24: 76) of perfluorooctane sulfonate is mobile phase;Detection wavelength is 277nm.Number of theoretical plate presses hydrochloric acid motherwort
Alkali peak is calculated and should be not less than 6000.
The preparation of reference substance solution takes hydrochloric acid leonurine reference substance in right amount, accurately weighed, plus 70% ethanol is made often
Solution of the 1ml containing 30ug, obtains final product.
Accurate absorption reference substance solution is each with need testing solution under stachydrine hydrochloride (assay) item respectively for determination method
10ul, notes people's liquid chromatograph, determines, and obtains final product.
Result judgement:This product is calculated by dry product, hydrochloric leonurine (C14H21O5N3HCl) must not be less than
0.044%.
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 motherwort 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
Residual quantity, and the standard limits of the stachydrine hydrochloride in assay are improved to 0.44%, hydrochloric acid leonurine from 0.40%
Standard limits improved to 0.044% from 0.040%.
2. the quality standard of the motherwort qualitative, quantitative prepared slices of Chinese crude drugs as described in claim 1, it is characterised in that:
Medicine bits impurity according to determination of foreign matter method (《Chinese Pharmacopoeia》Four general rules 2301 of version in 2015) determine (《Chinese Pharmacopoeia》2015
Four general rules of version hereinafter referred to as general rule), 3% should be crossed.
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.
Assay is determined according to high performance liquid chromatography (general rule 0512) determination method, and this product is calculated by dry product, hydrochloric wood
Alkali must not must not be less than 0.044% less than 0.44 (ml/g), hydrochloric leonurine.
3. the manufacturing process of the motherwort qualitative, quantitative prepared slices of Chinese crude drugs, it is characterised in that be prepared into the suitable motherwort prepared slices of Chinese crude drugs, wraps
Include following steps:
A10, net system:The impurity that is mixed in motherwort of removing and the product that go mouldy etc., to reach clean or to be processed further treatment.
A20, demulcen:Motherwort after net system is put into Xi Run ponds, water spray heap profit 16-24h, is thoroughly run through to motherwort.
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, motherwort 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
6-8h 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 medicinal material 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.
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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