CN106770880A - The quality standard and manufacturing process of the lamiophlomis rotata qualitative, quantitative prepared slices of Chinese crude drugs - Google Patents

The quality standard and manufacturing process of the lamiophlomis rotata qualitative, quantitative prepared slices of Chinese crude drugs Download PDF

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Publication number
CN106770880A
CN106770880A CN201610368266.0A CN201610368266A CN106770880A CN 106770880 A CN106770880 A CN 106770880A CN 201610368266 A CN201610368266 A CN 201610368266A CN 106770880 A CN106770880 A CN 106770880A
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lamiophlomis rotata
solution
product
crude drugs
prepared slices
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黄华强
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Guangzhou Jindian Jingfang Pharmaceutical Co Ltd
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Guangzhou Jindian Jingfang Pharmaceutical Co Ltd
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    • 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
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    • G—PHYSICS
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    • 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
    • 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
    • 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
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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
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
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    • 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
    • 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
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    • 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
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    • 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
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    • 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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    • 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
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Abstract

The invention provides one kind is safe efficient, the easily lamiophlomis rotata prepared slices of Chinese crude drugs.The lamiophlomis rotata qualitative, quantitative prepared slices of Chinese crude drugs manufacturing process that the present invention is provided, using a kind of processing procedure, the lamiophlomis rotata that procurement criteria will be met prepares the prepared slices of Chinese crude drugs, can brew and take change traditional decoction instructions of taking, there is provided a kind of lamiophlomis rotata quality standard simultaneously, increase coherent detection project on the basis of existing quality standard, and improve the standard limits of the total amount of the mountain Cape jasmine glycosides methyl esters in assay and 8 O acetyl mountain Cape jasmine glycosides methyl esters, quality that can be effectively to lamiophlomis rotata is controlled, the quality standard of medicine is improve, drug safety is increased.

Description

The quality standard and manufacturing process of the lamiophlomis rotata qualitative, quantitative prepared slices of Chinese crude drugs
Technical field
The present invention relates to the field of Chinese medicines, specially the quality standard of the lamiophlomis rotata qualitative, quantitative prepared slices of Chinese crude drugs, operational procedure with Manufacturing process.
Background technology
Lamiophlomis rotata (scientific name：Lamiophlomis rotata (Benth.) Kudo) alias：Bus, cloth bar is beaten, be Labiatae Plant.Lamiophlomis rotata is containing cyanidenon, cyanidenon -7-O- glycosides, Quercetin, Quercetin -3-O- Arab glucoside, quercitrin Element, Quercetin -3-O- Arab glucoside, apiolin -7-O- new dried orange peels glucoside, cupreol, palmitic acid, lamiophlomiol shanzhiside first Ester, 8-O- acetyl group shanzhisides methyl esters, flax belong to the active ingredients such as glucoside, and its function is used with to cure mainly be promoting blood circulation and hemostasis, wind-expelling pain-stopping In traumatic injury, traumatism and bleeding, arthralgia pain due to rheumatism, grasserie.Lamiophlomis rotata as conventional Chinese medicine, 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 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).Raw medicinal material Due to natural causes such as soil, plant evolutions, or spray insecticide or be contaminated by artificial origins such as Industrial " three Waste "s, so that Medicinal material is caused to contain heavy metal；Or the matter such as it is contaminated and causes heavy metals exceeding standard, residues of pesticides exceeded in Chinese medicine collection, transport Amount problem (golden saussurea involucrata, heavy metals pollution in Chinese medicine source and control measure research【J】Square medicine _ study of pharmacy, 2011).
Brief description of the drawings
Accompanying drawing 1 is lamiophlomis rotata 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 lamiophlomis rotata qualitative, quantitative prepared slices of Chinese crude drugs that the present invention is provided Skill, increases to medicine bits impurity, heavy metal and harmful element, Residual Levels of Organochlorine Pesticides, AFB1, sulfur dioxide residue The detection of amount, and by the standard limits of the mountain Cape jasmine glycosides methyl esters in assay and the total amount of 8-O- acetyl mountain Cape jasmine glycosides methyl esters from 0.50% improves to 0.55%.And the lamiophlomis rotata prepared slices of Chinese crude drugs are produced by specific operation, it is ensured that the prepared slices of Chinese crude drugs meet high standard Quasi- quality requirements.
The manufacturing process of the lamiophlomis rotata 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 lamiophlomis rotata of removing and the product that go mouldy etc., leaf is torn from petiole, makes it with original Medicinal material is separated, to reach clean or to be processed further processing.Note：Lamiophlomis rotata must not directly contact ground after cleaning.
A20, cleaning：Lamiophlomis rotata is placed in wash pond after net system, is cleaned up to without silt, quickly to be robbed during cleaning Wash, reduce lamiophlomis rotata soak time in water.
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, lamiophlomis rotata 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, 55 ± 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 lamiophlomis rotata for weighing predetermined weight are put into hopper, are sealed with sealing machine, it is desirable to accomplish Sealing external packing tight, smooth, attractive in appearance：Adjusted in equipment the date of manufacture and lot number that need to be printed, QA monitoring, in external packing Lot number, date of manufacture are printed on box, should be noted whether lot number and date of manufacture are clear in print procedure.After the completion of inner packing Medicine materical crude slice and survey report be put into outsourcing box, 4 bags/box.Every 10 box medicine materical crude slice is inserted in 1 heat shrinkage film, carries out hot receipts Contracting；It is fitted into after thermal contraction in big carton, 240 boxes/case.In operating process, QA is inspected by random samples at any time.Post personnel need to fill in into after packaging Product please examine list, hand over Quality Mgmt Dept to carry out product examination by QA samplings.
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 to medicine bits impurity, heavy metal and harmful element, Residual Levels of Organochlorine Pesticides, AFB1, titanium dioxide The detection of sulphur residual quantity, and by the mountain Cape jasmine glycosides methyl esters in assay and the standard limits of the total amount of 8-O- acetyl mountain Cape jasmine glycosides methyl esters Improved to 0.55% from 0.50%.The quality standard of the revised lamiophlomis rotata qualitative, quantitative prepared slices of Chinese crude drugs is as follows：
Lamiophlomis rotata medicine materical crude slice
Phonetic title：Duyiwei Yinpian
Packaging：Fine aluminium composite film packaging.
【Proterties】Take this product appropriate, observe in the sunlight, this product smells it in irregular broken, and gas is micro-, tastes it, taste micro-puckery, It is bitter.
Differentiate
Microscopical characters
Instrument and apparatus：Medicinal herb grinder, pharmacopeia sieve, microscope, alcolhol burner
Reagent and test solution：(reagent is used and divided for chloraldurate test solution, glycerine acetic acid test solution, glycerol-alcohol test solution, dilute glycerine Analysis is pure, and experimental water is purified water)
Determine and result judgement
In right amount, picking is put on slide a little, and glycerine acetic acid test solution, chloraldurate is added dropwise to take this product powder (crossing No. four sieves) Test solution or other test solutions 1~2 drip, covered.After chloraldurate test solution is added dropwise if necessary, saturatingization is heated on alcolhol burner, And glycerol-alcohol test solution or dilute glycerine, covered, in basis of microscopic observation is added dropwise：This product powder sepia.Nonglandular hair is many It is many, 2~3 cells composition, 10~15 μm of diameter, wall is thicker, there is verruca.Mesophyll cell is in irregular shape, includes numerous grass Sour calcium needle, it is long 7~10 μm.Stomata diacytic type or inequality.Fiber spindle shape, cinclides transverse fissure.
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, chloroform, methyl alcohol (reagent is pure using analysis)
Control medicinal material and reference substance：Lamiophlomis rotata control medicinal material, mountain mast glycosides methyl esters reference substance, 8-O- acetyl mountain Cape jasmine glycosides methyl esters pair According to product
Determine and result judgement
This product powder 1g, plus ethanol 10ml are taken, is heated to reflux 15 minutes, filtered, take filtrate as need testing solution.Separately take Lamiophlomis rotata control medicinal material 1g, is made in the same way of control medicinal material solution.Mountain mast glycosides methyl esters reference substance, 8-O- acetyl mountain Cape jasmine glycosides methyl esters are taken again Reference substance, plus ethanol is made every 1ml respectively mixed solutions containing 0.5mg, used as reference substance solution.According to thin-layered chromatography (general rule 0502) test, draw the μ l of need testing solution 5~10, control medicinal material solution and each 5 μ l of reference substance solution, put respectively in same silicon On glue G lamellaes, with chloroform-methyl alcohol (4: 1) as solvent, launch, take out, dry, spray with phosphomolybdic acid test solution, 105 It is clear DEG C to be heated to spot development.
Result judgement：In test sample chromatogram, on position corresponding with control medicinal material chromatogram and reference substance chromatogram, show identical The spot of color.
Check
Medicine bits, impurity
Instrument and apparatus：Medicinal herb grinder, assay balance, pharmacopeia sieve
Test sample about 100g (being accurate to 0.1g) is taken, is spread out, sort out impurity, sifted out medicine with No. 6 and consider to be worth doing, merged, weighed, counted Calculate its amount (%) in test sample.
Result judgement：This product medicine bits, impurity must not cross 3%.
Moisture
Instrument and apparatus：Medicinal herb grinder, assay balance, pharmacopeia sieve, electric heating constant-temperature blowing drying box, measuring cup
Determine and result judgement：Determined according to aquametry (method of general rule 0,832 second).
2~5g of test sample is taken, is laid in and is dried into the flat measuring cup of constant weight, thickness is no more than 5mm, loose test sample Accurately weighed no more than 10mm, open bottle cover covers bottle cap in 100~105 DEG C of dryings 5 hours, in dislocation drier, puts It is cold 30 minutes, accurately weighed, then dried 1 hour in said temperature, let cool, weigh, it is no more than to the double difference weighed Untill 5mg.According to the weight of less loss, water content (%) in test sample is calculated.
Result judgement：This product moisture must not cross 13.0%.
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 13.0%.
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 (reagent is pure using analysis, and experimental water is 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 4.0%.
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, rufous is slowly heated in 120 DEG C Steam is waved to the greatest extent, and continues to be concentrated into 2~3ml, is let cool, plus 20% sulfuric acid solution 2ml, 5% liquor potassic permanganate 0.5ml, is shaken up, 5% hydroxylamine hydrochloride solution to aubergine is added dropwise just to disappear, is transferred in 10ml measuring bottles, wash container with water, washing lotion is incorporated in measuring bottle In, and scale is diluted to, and shake up, it is centrifuged if necessary, supernatant is taken, obtain final product.With method while reagent preparation blank solution.
Determination method is accurate to draw that blank solution is appropriate with need testing solution, the method under sighting target directrix curve preparation determine from The content of mercury (Hg) in need testing solution is read on standard curve, is calculated, obtained final product.
Cupper determination (flame method)
Condition determination Detection wavelength is 324.7nm, using Air-acetylene Flame, background correction is carried out if necessary.
The preparation precision of copper Standard Reserving Solution measures copper single element standard liquid in right amount, is diluted with 2% salpeter solution, is made Solution per 1ml cupric (Cu) 10 μ g, obtains final product (0~5 DEG C of storage).
Precision measures copper Standard Reserving Solution in right amount respectively for the preparation of standard curve, and every 1ml difference is made of 2% salpeter solution The μ g of cupric 0,0.05 μ g, 0.2 μ g, 4 μ g, 0.6 μ g, the solution of 0.8 μ g.Flame is sprayed into successively, and mensuration absorbance is with absorbance Ordinate, concentration is abscissa, draws standard curve.
The preparation of need testing solution determines the preparation of need testing solution under item with lead.
Determination method is accurate to draw blank solution with need testing solution in right amount, and the method under the preparation of sighting target directrix curve is surveyed It is fixed.The content of copper (Cu) from need testing solution is read on standard curve, calculates, and obtains final product.
Result judgement：This product is leaded must not cross 8mg/kg, cadmium must not cross 0.8mg/kg, arsenic must not cross 4mg/kg, mercury must not Crossing 0.8mg/kg, copper must not cross 20mg/kg.
Organic chlorine agriculture chemicals residual quantity
Instrument and apparatus：Medicinal herb grinder, assay balance, pharmacopeia sieve, Rotary Evaporators, supersonic wave cleaning machine, gas phase color Spectrometer
Reagent and test solution：Petroleum ether (60~90 DEG C), acetone, sodium chloride, dichloromethane, anhydrous sodium sulfate (its petrochina (60~90 DEG C) of ether is chromatographically pure, and other reagents are pure using analysis, and experimental water is purified water)
Reference substance：α-BHC, β-BHC, γ-BHC, δ-BHC, 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, 8-BHC sums) containing total BHC must not cross 0.2mg/kg； Total DDT (pp '-DDE, pp '-DDD, op '-DDT, pp '-DDT sums) must not cross 0.2mg/kg；Pentachloronitrobenzene must not mistake 0.1mg/kg。
AFB1
Instrument and apparatus：Medicinal herb grinder, assay balance, pharmacopeia sieve, homogeneous bottle, centrifuge, high performance liquid chromatograph (are matched somebody with somebody Put fluorescence detector and derivatization pump, derivatization incubator)
Reagent and test solution：(wherein acetonitrile is chromatographically pure, and other reagents are for methyl alcohol, acetonitrile, iodine, sodium chloride, immune affinity column Analysis is pure, and experimental water is purified water)
Reference substance：AFB1Reference substance
Method：Determined according to aflatoxin determination method (general rule 2351).
Chromatographic condition is with system suitability with octadecylsilane chemically bonded silica as filler；With methanol-acetonitrile-water (40: 18: 42) are mobile phase；Detected using post-column derivation method, iodine derivatization method：Derivative solution is that 0.05% iodine solution (takes iodine 0.5g, adds methyl alcohol 100ml to make dissolving, is diluted with water to 1000ml and is made), derivatization flow rate pump 0.3ml per minute, derivatization Temperature 70 C is with fluorescence detector detection, excitation wavelength lambda ex=360nm (or 365nm), emission wavelength lambda ex=450nm.Two The separating degree of adjacent chromatographic peak should be greater than 1.5.
The preparation precision of mixed reference substance solution measures AFB1(sign concentration is 1.0 μ g/ to reference substance solution Ml) 0.5ml, in putting 10ml measuring bottles, with methanol dilution to scale, as stock solution.Precision measures stock solution 1ml, puts In 25ml measuring bottles, with methanol dilution to scale, obtain final product.
The preparation of need testing solution takes test sample powder about 15g (crossing No. two sieves), accurately weighed, is placed in homogeneous bottle, plus Enter sodium chloride 3g, precision adds 70% methanol solution 75ml, 2 minutes (mixing speed is more than 11000 revs/min) of high-speed stirred, 5 minutes (2500 revs/min of centrifugal speed) of centrifugation, precision measures supernatant 15ml, puts in 50ml measuring bottles, is diluted with water to quarter Degree, shakes up, and with (0.45 μm) filtration of miillpore filter, measures subsequent filtrate 20.0ml, by immune affinity column, flow velocity 3ml per minute, Eluted with water 20ml, eluent is discarded, and admits air into pillar, water is extruded into pillar, then eluted with proper amount of methanol, collect wash-out Liquid, in putting 2ml measuring bottles, and with methanol dilution to scale, shakes up, and obtains final product.
Determination method is accurate respectively to draw the above-mentioned μ l of mixed reference substance solution 5,10 μ l, 15 μ l, 20 μ l, 25 μ l, injects liquid phase Chromatograph, determines peak area, and with peak area as ordinate, sample size is abscissa, draws standard curve.Another accurate absorption is above-mentioned The μ l of need testing solution 20~25, inject liquid chromatograph, determine peak area, equivalent to Huang from test sample is read on standard curve Aspertoxin B1Amount, calculate, obtain final product.
Result judgement：This product must not cross 5 μ g per 1000g containing AFB1.
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 (0.0lmol/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, with 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 oneself and dries in 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 20%.
Assay
Instrument and apparatus：Medicinal herb grinder, assay balance, pharmacopeia sieve, thermostat water bath, high performance liquid chromatograph
Reagent and test solution：(wherein acetonitrile is chromatographically pure, and other reagents are pure using analysis, real for acetonitrile, methyl alcohol, purified water It is purified water to test with water)
Reference substance：Mountain Cape jasmine glycosides methyl esters reference substance, 8-O- acetyl mountain Cape jasmine glycosides methyl esters reference substances
Determine and result judgement：Determined according to high performance liquid chromatography (general rule 0512).
Chromatographic condition is with system suitability with octadecylsilane chemically bonded silica as filler；It is flowing with acetonitrile Phase A, water is Mobile phase B, and the regulation according to the form below carries out gradient elution；Detection wavelength is 235nm.Number of theoretical plate presses mountain Cape jasmine glycosides first Ester peak is calculated and should be not less than 3000.
The preparation of reference substance solution takes mountain Cape jasmine glycosides methyl esters reference substance, 8-O- acetyl mountain Cape jasmine glycosides methyl esters reference substance in right amount, accurate It is weighed, plus methyl alcohol be made every 1ml respectively containing 30 μ g mixed solution, obtain final product.
The preparation of need testing solution takes this product powder (cross No. three sieve) about 0.6g, accurately weighed, in putting conical flask with cover, Precision adds 70% methyl alcohol 25ml, and close plug, weighed weight is heated to reflux 1 hour, lets cool, then weighed weight, is mended with 70% methyl alcohol The weight of sufficient less loss, shakes up, filtration, and precision measures subsequent filtrate 2ml, and in putting 10ml measuring bottles, plus methyl alcohol is to scale, shakes up, filtration, Subsequent filtrate is taken to obtain final product.
Determination method is accurate respectively to draw reference substance solution and each 10 μ l of need testing solution, injects liquid chromatograph, determines, Obtain final product.
Result judgement：This product is calculated by dry product, the methyl esters of glycosides containing mountain Cape jasmine (C17H26O11) and 8-O- acetyl mountain Cape jasmine glycosides methyl esters (C19H28O12) total amount must not be less than 0.55%.
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 lamiophlomis rotata 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 by the standard limits of the mountain Cape jasmine glycosides methyl esters in assay and the total amount of 8-O- acetyl mountain Cape jasmine glycosides methyl esters from 0.50% Improve to 0.55%.
2. the quality standard of the lamiophlomis rotata qualitative, quantitative prepared slices of Chinese crude drugs as described in claim 1, it is characterised in that：
Medicine is considered impurity to be worth doing and is determined according to determination of foreign matter method (general rule 2301), should cross 3%.
Heavy metal and harmful element are determined according to lead, cadmium, arsenic, mercury, copper determination method (general rule 2321), and this product is leaded must not to cross 8mg/ Kg, cadmium must not cross 0.8mg/kg, arsenic and must not cross 4mg/kg, mercury and must not cross 0.8mg/kg, copper and must not cross 20mg/kg.
Residual Levels of Organochlorine Pesticides according to persticide residue determination method (method of general rule 0,512 first) determine, this product containing total BHC (α- BHC, β-BHC, γ-BHC, δ-BHC sums) must not cross 0.2mg/kg, total DDT (pp '-DDE, pp '-DDD, op '-DDT, Pp '-DDT sums) 0.2mg/kg, pentachloronitrobenzene must not be crossed 0.1mg/kg must not be crossed.
AFB1Determined according to aflatoxin determination method (general rule 2351), this product contains AFB15 μ g/ must not be crossed kg。
Sulfur dioxide residual quantity is determined according to sulfur dioxide residual quantity determination method (general rule 2331), and this product sulfur dioxide residual quantity must not Cross 150mg/kg.
3. the manufacturing process of the lamiophlomis rotata qualitative, quantitative prepared slices of Chinese crude drugs, it is characterised in that prepare the lamiophlomis rotata prepared slices of Chinese crude drugs, including with Lower step：
A10, net system：The impurity that is mixed in lamiophlomis rotata of removing and the product that go mouldy etc., leaf is torn from petiole, makes itself and crude drug Separate, to reach clean or to be processed further processing.Note：Lamiophlomis rotata must not directly contact ground after cleaning.
A20, cleaning：Lamiophlomis rotata is placed in wash pond after net system, is cleaned up to without silt, and Rapid Cleaning is wanted during cleaning, is subtracted Few lamiophlomis rotata soak time in water.
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, lamiophlomis rotata 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, 55 ± 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 lamiophlomis rotata for weighing predetermined weight are put into hopper, are sealed with sealing machine, it is desirable to accomplish sealing Tightly, external packing smooth, attractive in appearance：Adjusted in equipment the date of manufacture and lot number that need to be printed, QA monitoring, in external packing cases Upper printing lot number, date of manufacture, should be noted whether lot number and date of manufacture are clear in print procedure.By the drink after the completion of inner packing Piece and survey report are put into outsourcing box, 4 bags/box.Every 10 box medicine materical crude slice is inserted in 1 heat shrinkage film, carries out thermal contraction；Heat It is fitted into after contraction in big carton, 240 boxes/case.In operating process, QA is inspected by random samples at any time.Post personnel need to fill in finished product and ask after packaging Inspection is single, hands over Quality Mgmt Dept to carry out product examination by QA samplings.
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.
CN201610368266.0A 2016-05-21 2016-05-21 The quality standard and manufacturing process of the lamiophlomis rotata qualitative, quantitative prepared slices of Chinese crude drugs Pending CN106770880A (en)

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