CN106706827A - Quality standard and manufacturing process of barbed skullcap herb qualitative and quantitative traditional Chinese medicine decoction pieces - Google Patents

Quality standard and manufacturing process of barbed skullcap herb qualitative and quantitative traditional Chinese medicine decoction pieces Download PDF

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Publication number
CN106706827A
CN106706827A CN201610368024.1A CN201610368024A CN106706827A CN 106706827 A CN106706827 A CN 106706827A CN 201610368024 A CN201610368024 A CN 201610368024A CN 106706827 A CN106706827 A CN 106706827A
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sculellaria barbata
solution
product
standard
decoction pieces
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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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    • 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
    • G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
    • 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
    • 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
    • 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
    • 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
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • 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
    • 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
    • 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
    • G01N2021/3114—Multi-element AAS arrangements
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N2021/3129—Determining multicomponents by multiwavelength light
    • 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
    • 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
    • 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
    • G01N2030/062—Preparation extracting sample from raw material
    • 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
    • G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
    • G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample

Abstract

The invention provides safe, efficient and convenient barbed skullcap herb traditional Chinese medicine decoction pieces, and a manufacturing process of barbed skullcap herb qualitative and quantitative traditional Chinese medicine decoction pieces. A processing process is adopted, barbed skullcap herb meeting quality standards is prepared into the traditional Chinese medicine decoction pieces, the traditional Chinese medicine decoction pieces can be brewed to be taken, and a traditional decocting taking method is changed. Meanwhile, a quality standard of the barbed skullcap herb decoction pieces is provided. Relevant detection items are added on the basis of an existing quality standard, the standard limit of total flavonoid glycoside and terpene lactone in content measurement is improved, the quality of the barbed skullcap herb decoction pieces can be effectively controlled, the quality standard of medicine is improved, and pharmacy safety is improved.

Description

The quality standard and manufacturing process of the Sculellaria barbata 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 Sculellaria barbata qualitative, quantitative prepared slices of Chinese crude drugs, operational procedure with Manufacturing process.
Background technology
Sculellaria barbata (scientific name：Scutellaria barbata D.Don), alias Herba hyperici attenuati, the thin root of large-flowered skullcap, toothbrush grass, Tian Ji Grass, the water root of large-flowered skullcap, narrow leaf indian skullcap herb with root, are lamiaceae labiatae scutellaria herbaceos perennials.Sculellaria barbata as conventional Chinese medicine, with powerful Potentiality to be exploited.Sculellaria barbata is containing carthamin, isocarthamidin, high mountain baicalein, high mountain Huang official seal glucoside, cupreol, stearic acid, biology Alkali polysaccharide, wogonin, rivularin, Sculellaria barbata kind element, naringenin, apiolin, dinatin, eriodictyol, cyanidenon, P-coumaric acid, protocatechuic acid, can tartaric acid, phytosterol, phytosterol β-D-Glucose glucoside etc. active ingredient, its function with It is clearing heat and detoxicating, stagnation resolvation diuresis to cure mainly, and for furuncle swelling toxin, abscess of throat, the pain of injury caused by falling and tumbling, oedema, jaundice, snake bite and insect sting, is fallen Flutter and swell and ache and oedema/jaundice etc..The master thesis of Wang Ping《The research of Sculellaria barbata anticancer component》Point out that " Sculellaria barbata is near several Year domestic and international one of study hotspot of antineoplastic.Modern pharmacological research shows that Sculellaria barbata water extract and alcohol extract are antineoplastic Mechanism of action mainly includes：Directly suppress tumour growth with proliferation function, inducing apoptosis of tumour cell effect, anti-oxidant anti-freedom Base effect etc..", and Isorhamnetin and Quercetin in Sculellaria barbata ethyl acetate layer extract are determined by experiment with suppression blood Pipe generation activity.Geng Xianyu's etc.《The exploration of Scutellaria barbata antitumor action and discovery》The antitumor research of Sculellaria barbata is carried out Summary.
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.
To be solved by this invention is the generally existing unconspicuous problem of prepared slices of Chinese crude drugs curative effect in the market.Chinese medicine big gun The factors such as system and formulation, the compatibility of Chinese medicine, dosage, method of administration, allotment, decoction method, the diet of Chinese medicine are equal to Chinese Herbs Have a significant effect (the factor of Liu Hongxing, fourth tree simple analysis influence Chinese Herbs【J】Traditional Chinese medicine, 2014).Chinese medicine is because of ring The heavy metals exceeding standard that the problems such as border is polluted causes；Largely using for agricultural chemicals brings Pesticide Residue to Sculellaria barbata aborning, and Organo-chlorine pesticide is more very slow because of its degradation speed, is widely present in the environment, and is accumulated in food chain, influences the health of people (Residual Levels of Organochlorine Pesticides detection in the Sculellaria barbatas such as Yu Minqian【J】Chinese medicine, 2002) quality such as cause residues of pesticides exceeded Problem.
Brief description of the drawings
Accompanying drawing 1 is Sculellaria barbata 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 Sculellaria barbata 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 it is residual The detection of allowance, and the general flavone in assay is contained into general flavone (with scutellarin C21H18O12Meter) standard limits from 1.50% is improved to 1.65%, and scutellarin standard limits are improved to 0.22% from 0.20%.And produced by specific operation Go out the Sculellaria barbata prepared slices of Chinese crude drugs, it is ensured that the prepared slices of Chinese crude drugs meet the requirement of high standard high-quality.
The manufacturing process of the Sculellaria barbata 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 Sculellaria barbata of removing and the product that go mouldy etc., to reach clean or to be processed further place Reason.Note：Sculellaria barbata must not directly contact ground after cleaning.
A20, cleaning：Sculellaria barbata is placed in wash pond after net system, is cleaned up to without silt, quickly clear during cleaning Wash, reduce Sculellaria barbata soak time in water, heap profit 6-8h, thoroughly runs through to Sculellaria barbata after the completion of cleaning.
A30, cutting：Operated by fully automatic high-speed slicer operational procedure, mix up knife away from 0.4mm, carry out cutting medicine.
A40, drying：It is dried using heated-air circulation oven, Sculellaria barbata is laid on baking oven shelf, paving thickness is equal Even, thickness is in below 3cm.Switch is opened, heater switch, blower fan is opened, 60 ± 2 DEG C are dried in temperature, are reached in temperature 5-7h is dried after design temperature, drying is finished, and closes heater switch, continue to dry, treat that the temperature inside the box is fallen to 35~40 DEG C, closed Close blower fan.Post personnel need to fill in intermediate products and please examine list after drying, hand over Quality Mgmt Dept to carry out moisture inspection by QA samplings.
A50, packaging：Packed according to the requirement of this product packing specification.Need to check make-up room before packaging, confirm bag Clearing out a gathering place for assembling production lines has been completed, and checks whether packaging material meet the requirements.Inner packing：Being adjusted in equipment needs print The date of manufacture of system, lot number, QA monitoring, the Sculellaria barbata for weighing predetermined weight are put into hopper, are sealed with sealing machine, it is desirable to accomplish Sealing is tight, smooth, attractive in appearance.External packing：Adjusted in equipment the date of manufacture and lot number that need to be printed, QA monitoring, in outsourcing Lot number, date of manufacture are printed on mounted box, should be noted whether lot number and date of manufacture are clear in print procedure.Inner packing is completed Medicine materical crude slice and survey report afterwards is put into outsourcing box, 4 bags/box.Every 10 box medicine materical crude slice is inserted in 1 heat shrinkage film, carries out hot receipts Contracting；It is fitted into after thermal contraction in big carton, 240 boxes/case.In operating process, QA is inspected by random samples at any time.Post personnel need to fill in into after packaging Product please examine list, hand over Quality Mgmt Dept to carry out product examination by QA samplings.
A60, finished product：Post personnel need to fill in finished product and please examine list after packaging, hand over Quality Mgmt Dept to carry out product examination by QA samplings.
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 the general flavone in assay is contained into general flavone (with scutellarin C21H18O12Meter) standard limits Improved to 1.65% from 1.50%, scutellarin standard limits are improved to 0.22% from 0.20%.Revised Sculellaria barbata is qualitative The quality standard of the quantitative prepared slices of Chinese crude drugs is as follows：
Sculellaria barbata medicine materical crude slice
Phonetic title：Banzhilian 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, taste is micro- It is bitter.
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, medication is sifted out medicine bits, merged, weigh, counts Calculate its amount (%) in test sample
Result judgement：This product 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 12.0%.
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；1700~2100 DEG C of atomization temperature, continues 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, 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, 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 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 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 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, it is careful to add Enter sulfuric acid 1ml, shake 1 minute, centrifugation (3000 revs/min) 10 minutes, precision measures supernatant 2ml, puts the concentration of tool scale In 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。
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：AFB] reference substance
Method：Determined according to aflatoxin determination method (general rule 2351).
Chromatographic condition is with system suitability with octadecylsilane chemically bonded silica as filler；With methanol-acetonitrile-water (40: 18: 42) are mobile phase；Detected using post-column derivation method, iodine derivatization method：Derivative solution is that 0.05% iodine solution (takes iodine 0.5g, adds methyl alcohol 100ml to make dissolving, is diluted with water to 1000ml and is made), derivatization flow rate pump 0.3ml per minute, derivatization Temperature 70 C is with fluorescence detector detection, excitation wavelength lambda ex=360nm (or 365nm), emission wavelength lambda ex=450nm.Two The separating degree of adjacent chromatographic peak should be greater than 1.5.
The preparation precision of mixed reference substance solution measures AFB1(sign concentration is 1.0 μ g/ to reference substance solution Ml) 0.5ml, in putting 10ml measuring bottles, with methanol dilution to scale, as stock solution.Precision measures stock solution 1ml, puts In 25ml measuring bottles, with methanol dilution to scale, obtain final product.
The preparation of need testing solution takes test sample powder about 15g (crossing No. two sieves), accurately weighed, is placed in homogeneous bottle, adds chlorine Change sodium 3g, precision adds 70% methanol solution 75ml, 2 minutes (mixing speed is more than 11000 revs/min) of high-speed stirred, centrifugation 5 Minute (2500 revs/min of centrifugal speed), precision measures supernatant 15ml, puts in 50ml measuring bottles, is diluted with water to scale, shakes It is even, with (0.45 μm) filtration of miillpore filter, subsequent filtrate 20.0ml is measured, by immune affinity column, flow velocity 3ml per minute uses water 20ml is eluted, and eluent is discarded, and admits air into pillar, and water is extruded into pillar, then is eluted with proper amount of methanol, collects eluent, In putting 2ml measuring bottles, and with methanol dilution to scale, shake up, obtain final product.
Determination method is accurate respectively to draw the above-mentioned μ l of mixed reference substance solution 5,10 μ l, 15 μ l, 20 μ l, 25 μ l, injects liquid phase Chromatograph, determines peak area, and with peak area as ordinate, sample size is abscissa, draws standard curve.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 The amount of AFB1, calculates, and obtains final product.
Result judgement：This product contains AFB per 1000g15 μ g must not be crossed.
Sulfur dioxide residual quantity
Instrument and apparatus：Medicinal herb grinder, assay balance, pharmacopeia sieve, electric jacket
Reagent and test solution：Hydrogen peroxide, methyl red ethanol solution, 0.01mol/L sodium hydroxide titrations liquid, hydrochloric acid solution (6mol/L) (reagent is pure using analysis, and experimental water is purified water)
Method：Determined according to sulfur dioxide residual quantity determination method (general rule 2331).Get it filled material or medicine materical crude slice fine powder about 10g, accurate It is weighed, put in two neck round-bottom flasks, add water 300~400ml.Reflux condensing tube switch feedwater is opened, by upper end E mouthfuls of condenser pipe Place's one rubber wireway of connection is placed in 100ml conical flasks bottom.3% hydrogenperoxide steam generator 50ml is added in conical flask as absorption Liquid (end of rubber wireway should be below absorbing liquid liquid level).Using preceding, 3 are added to drip methyl red ethanol solution in absorbing liquid Indicator (2.5mg/ml), and it is titrated to yellow (i.e. terminal with 0.01mol/L sodium hydroxide titration liquid；If it exceeds terminal, then The absorbent solution should be given up).Nitrogen is opened, flowmeter adjusting gas flow to about 0.2L/min is used；Open separatory funnel C's Piston, makes hydrochloric acid solution (6mol/L) 10ml flow into cucurbit, is immediately heated the solution in two neck flasks to boiling, and keep micro- Boiling；Boiling water in flask stops heating after 1.5 hours.After absorbing liquid lets cool, it is placed on magnetic stirring apparatus and is stirred continuously, uses Sodium hydroxide titration liquid (0.01mol/L) is titrated, and is not taken off within 20 seconds to the yellow duration, and by the result blank assay of titration Correction.
Result judgement：This product sulfur dioxide residual quantity must not cross 150mg/kg.
General flavone
Instrument and apparatus：Medicinal herb grinder, assay balance, pharmacopeia sieve, thermostat water bath, ultraviolet-uisible spectrophotometer
Reagent and test solution：Methyl alcohol (reagent is pure using analysis, and experimental water is two grades of water)
Reference substance：Scutellarin reference substance
Determine and result judgement：According to UV-VIS spectrophotometry (general rule 0401)
The preparation of reference substance solution takes scutellarin reference substance in right amount, accurately weighed, plus methyl alcohol is made every 1ml containing 0.2mg Solution, obtain final product.
The preparation precision of standard curve measures reference substance solution 0.4ml, 0.8ml, 1.2ml, 1.6ml, 2.0ml and puts respectively In 25ml measuring bottles, plus methyl alcohol is to scale, shakes up.With methyl alcohol as blank, according to UV-VIS spectrophotometry (general rule 0401), Mensuration absorbance is distinguished at the wavelength of 335nm, with absorbance as ordinate, concentration is abscissa, draw standard curve.
Determination method precision measure under [assay] item scutellarin through surname extraction and be diluted to 100ml methyl alcohol it is molten Liquid 1ml, in putting 50ml measuring bottles, plus methyl alcohol is to scale, shakes up, method under sighting target directrix curve preparation, from " with methyl alcohol as blank " Rise, in accordance with the law mensuration absorbance, the weight (mg) of scutellarin from need testing solution is read on standard curve is calculated, and is obtained final product.
This product is calculated by dry product, containing general flavone with scutellarin (C21H18O12) meter, 1.65% must not be less than.
Scutellarin
Instrument and apparatus：Medicinal herb grinder, assay balance, pharmacopeia sieve, thermostat water bath, high performance liquid chromatograph
Reagent and test solution：(wherein methyl alcohol is chromatographically pure, and other reagents are pure using analysis, real for acetic acid, methyl alcohol, purified water It is two grades of water to test with water)
Reference substance：Scutellarin reference substance
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；With methanol-water-acetic acid (35: 61: 4) are mobile phase；Detection wavelength is 335nm.Number of theoretical plate is calculated by scutellarin peak and should be not less than 1500.
The preparation of reference substance solution takes scutellarin reference substance in right amount, accurately weighed, plus mobile phase is made every 1ml containing 80 μ g Solution, obtain final product.
The preparation of need testing solution takes this product powder (cross No. three sieve) about 1g, accurately weighed, in putting apparatus,Soxhlet's, plus stone (60~90 DEG C) of oily ether is extracted to colourless, discards ether liquid, and the dregs of a decoction fling to petroleum ether, plus methyl alcohol continues to extract to colourless, is transferred to In 100ml measuring bottles, plus methyl alcohol is to scale, shakes up, and precision measures 25ml, is evaporated, and residue is dissolved with 20% methyl alcohol, is transferred to 25ml In measuring bottle, and scale is diluted to, shaken up, filtered, take subsequent filtrate, obtained final product.
Determination method is accurate respectively to draw reference substance solution and each 10 μ l of need testing solution, injects liquid chromatograph, determines, i.e., .
This product is calculated by dry product, containing scutellarin (C21H18O12) 0.22% must not be less than.
Microbial limit
Detection of Salmonella takes this product 10g, with the pancreas junket soybean of aseptic inoculation to appropriate volume (tested through method applicability and determined) In peptone fluid nutrient medium, mix, by non-sterile product limit test of microbe：Control bacteria examination method is checked.
Result judgement：Detection of Salmonella must not be detected (10g).
Bile tolerance gram-negative bacteria takes this product, with aseptic pancreas junket soya peptone fluid nutrient medium as diluent, is made 1: 10 Test liquid, mixes, by non-sterile product limit test of microbe：Control bacteria examination method is checked.
Result judgement：Bile tolerance gram-negative bacteria should be less than 104cfu(1g)。

Claims (3)

1. the quality standard of the Sculellaria barbata 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 general flavone in assay (with scutellarin C21H18O12Meter) standard limits from 1.50% improve to 1.65%, scutellarin standard limits are improved to 0.22% from 0.20%.
2. the quality standard of the Sculellaria barbata 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.
3. the manufacturing process of the Sculellaria barbata qualitative, quantitative prepared slices of Chinese crude drugs, it is characterised in that prepare the Sculellaria barbata prepared slices of Chinese crude drugs, including with Lower step：
A10, net system：The impurity that is mixed in Sculellaria barbata of removing and the product that go mouldy etc., to reach clean or to be processed further treatment.Note Meaning：Sculellaria barbata must not directly contact ground after cleaning.
A20, cleaning：Sculellaria barbata is placed in wash pond after net system, is cleaned up to without silt, and Rapid Cleaning is wanted during cleaning, is subtracted Few Sculellaria barbata soak time in water, heap profit 6-8h, thoroughly runs through to Sculellaria barbata after the completion of cleaning.
A30, cutting：Operated by fully automatic high-speed slicer operational procedure, mix up knife away from 0.4mm, carry out cutting medicine.
A40, drying：It is dried using heated-air circulation oven, Sculellaria barbata is laid on baking oven shelf, paving thickness is uniform, it is thick Degree is in below 3cm.Switch is opened, heater switch, blower fan is opened, 60 ± 2 DEG C are dried in temperature, setting temperature is reached in temperature 5-7h is dried after degree, drying is finished, and closes heater switch, continue to dry, treat that the temperature inside the box is fallen to 35~40 DEG C, close wind Machine.Post personnel need to fill in intermediate products and please examine list after drying, hand over Quality Mgmt Dept to carry out moisture inspection by QA samplings.
A50, packaging：Packed according to the requirement of this product packing specification.Need to check make-up room before packaging, confirm packaging life Clearing out a gathering place for producing line has been completed, and checks whether packaging material meet the requirements.Inner packing：Being adjusted in equipment needs printing Date of manufacture, lot number, QA monitoring, the Sculellaria barbata for weighing predetermined weight are put into hopper, are sealed with sealing machine, it is desirable to accomplish sealing Tightly, it is smooth, attractive in appearance.External packing：Adjusted in equipment the date of manufacture and lot number that need to be printed, QA monitoring, in external packing box Lot number, date of manufacture are printed on son, should be noted whether lot number and date of manufacture are clear in print procedure.After the completion of inner packing Medicine materical crude slice and survey report are put into outsourcing box, 4 bags/box.Every 10 box medicine materical crude slice is inserted in 1 heat shrinkage film, carries out thermal contraction； It is fitted into after thermal contraction in big carton, 240 boxes/case.In operating process, QA is inspected by random samples at any time.Post personnel need to fill in finished product after packaging List please be examine, hands over Quality Mgmt Dept to carry out product examination by QA samplings.
A60, finished product：Post personnel need to fill in finished product and please examine list after packaging, hand over Quality Mgmt Dept to carry out product examination by QA samplings.
CN201610368024.1A 2016-05-21 2016-05-21 Quality standard and manufacturing process of barbed skullcap herb qualitative and quantitative traditional Chinese medicine decoction pieces Pending CN106706827A (en)

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Application publication date: 20170524