CN102429966B - A kind of concocting method without gallbladder Radix Aconiti Lateralis Preparata - Google Patents
A kind of concocting method without gallbladder Radix Aconiti Lateralis Preparata Download PDFInfo
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Abstract
The invention provides a kind of concocting method without gallbladder Radix Aconiti Lateralis Preparata or Radix Aconiti Lateralis Preparata, it comprises the following steps: a, get fresh mud Radix Aconiti Lateralis Preparata, cleans; Moderate heat keeps boiling to boil 10-20min; B, section, leaching drift 20-30min, 105 DEG C of-110 DEG C of temperature, normal pressure steams 2-10h; C, oven dry, to obtain final product.The present invention also provide this concocting method to prepare without gallbladder Radix Aconiti Lateralis Preparata or Radix Aconiti Lateralis Preparata, do not add in concocting process edible gallbladder bar.Present invention substantially reduces the content of calcium ion in processed product, magnesium ion, chloride ion and other metal ions, while ensure that clinical efficacy, reduce toxic and side effects, improve drug safety.
Description
Technical field
The present invention relates to a kind of without gallbladder Radix Aconiti Lateralis Preparata or Radix Aconiti Lateralis Preparata and concocting method thereof, belong to drug world.
Background technology
Radix Aconiti Lateralis Preparata is the processed goods of the daughter root of ranunculaceae plant Aconitum carmichjaelii Debx. Aconitum carmichaelii Debx., has recuperating depleted YANG and rescuing the patient from collapse, mends fire supporing yang, effect of dispersing cold for relieving pain, for YANG-depletion collapse, cold extremities faint pulse, sexual impotence cold womb, coldness and pain in the epigastrium, deficiency and coldness is vomited and diarrhoea, YIN-cold edema, yang deficiency diseases caused by exogenous pathogenic factor, arthralgia due to cold-dampnes is a kind of important Chinese crude drug.Because Radix Aconiti Lateralis Preparata toxicity is violent, doctor is in order to subtract its toxicity, improve clinical efficacy at all times, and its processing procedure method is particularly paid attention to.Radix Aconiti Lateralis Preparata is as parts of generic medicinal plants, and Radix Aconiti Lateralis Preparata or Radix Aconiti Lateralis Preparata are its decoction pieces in one of the most common specification of clinical practice.
Traditional concocting method of Radix Aconiti Lateralis Preparata is: get mud Radix Aconiti Lateralis Preparata, cleans, and immerses a few days in the aqueous solution of edible gallbladder bar, boil to the saturating heart together with immersion, pull out, water floats, the sheet of rip cutting Cheng Houyue 0.5cm, float with water logging again, make Radix Aconiti Lateralis Preparata dye Umber by toner, take out, steam to after there is pasta, gloss, be dried to half-dried, then dry or continue to dry.Radix Aconiti Lateralis Preparata, after water drift, by the heat treated of steaming and decocting, makes its toxic component diester-type alkaloids be hydrolyzed and becomes the less monoester alkaloid of toxicity, both destroyed toxic component, and do not affect again its heart tonifying composition, ensure that clinical efficacy while reaching Attenuation.[Lu Nan. Radix Aconiti Lateralis Preparata processing procedure method brief analysis. " practical tcm internal medicine magazine " .2010,24:98-100]
Traditional concocting method of Radix Aconiti Lateralis Preparata is: select mud Radix Aconiti Lateralis Preparata of uniform size, cleans, and immerses a few days in the aqueous solution of edible gallbladder bar, boils to the saturating heart together with immersion, pull out, peel off crust, the sheet of rip cutting Cheng Houyue 0.3cm, floats with water logging, take out, steam thoroughly, dry, practise and claim " Radix Aconiti Lateralis Preparata ".
But modern study proves, in Radix Aconiti Lateralis Preparata or the Radix Aconiti Lateralis Preparata course of processing, gallbladder bar used is containing a large amount of calcium ion, magnesium ion, chloride ion and other metal ions, and in current traditional concocting method, the content of calcium, magnesium, chloride ion is approximately respectively: 1.7%, 0.3%, 3.8%.Calcium, magnesium ion have strong corrosiveness to stomach, make the protein coagulating of human organ, and magnesium ion absorbed after can suppress cardiovascular and nervous system, to people, there is larger toxicity.Although mud Radix Aconiti Lateralis Preparata wants flowing water to take off gallbladder 5 ~ 6 times after gallbladder bar soaks, also can not take off gallbladder complete, more have lawless person, in Radix Aconiti Lateralis Preparata, pour into gallbladder bar in a large number and Radix Aconiti Lateralis Preparata is increased weight.Therefore, the Radix Aconiti Lateralis Preparata prepared by traditional concocting method or Radix Aconiti Lateralis Preparata toxic and side effects are comparatively large, and safety exists certain hidden danger.
Although many scholars have carried out continuous exploration in recent years, employ new technology and improved the processing technique of Radix Aconiti Lateralis Preparata.As Liu Huiru etc. adopts uniform test design method, the best processing procedure of optimization is that fresh Radix Aconiti Lateralis Preparata adds 0.1% gallbladder bar, and decoct with water 3 hours, float 2 days, steam 2 hours, concocted time can shorten 8 days; Hu Sumei etc. adopt saturated aqueous common salt to replace gallbladder bar liquid to concoct Radix Aconiti Lateralis Preparata, and this author thinks that Radix Aconiti Lateralis Preparata has to pass through long-time immersion and could reduce its toxicity; Said method complicated process of preparation, high to the requirement of equipment, and also these processing technique all do not have the checking through excessive production, can not meet large Production requirement.
Summary of the invention
Technical scheme of the present invention there is provided a kind of concocting method without gallbladder Radix Aconiti Lateralis Preparata or Radix Aconiti Lateralis Preparata, and it does not add gallbladder bar in concocting process.Another technical scheme of the present invention there is provided prepared by this concocting method without gallbladder Radix Aconiti Lateralis Preparata or Radix Aconiti Lateralis Preparata.
The invention provides a kind of concocting method without gallbladder Radix Aconiti Lateralis Preparata or Radix Aconiti Lateralis Preparata, it comprises the following steps:
A, get fresh mud Radix Aconiti Lateralis Preparata, clean; Moderate heat keeps boiling to boil 10-20min;
B, section, leaching drift 20-30min, floats to slice surface inviscid, and 105 DEG C of-110 DEG C of temperature, normal pressure steams 2-10h;
C, oven dry, to obtain final product.
Wherein, the steaming time described in b step is 8h.
Wherein, the drying means described in step c is 40 DEG C-70 DEG C dries 17h-73h.
Wherein, the drying means described in step c is 55 DEG C dries 24h.
Wherein, the described concocting method without gallbladder Radix Aconiti Lateralis Preparata is: peelling off crust after boiling, cutting vertical sheet thickness is 0.3cm-0.5cm.
Wherein, the described concocting method without gallbladder Radix Aconiti Lateralis Preparata is: not peeling after boiling, cut vertical sheet, and thickness is 0.3cm-0.5cm.
Present invention also offers prepared by described concocting method without gallbladder Radix Aconiti Lateralis Preparata or Radix Aconiti Lateralis Preparata.
It contains monoester alkaloid with Benzoylmesaconine (C
31h
43nO
10), benzoyl aconine (C
32h
45nO
10) and benzoyl hypo-aconine (C
31h
43nO
9) total amount, must not 0.010% be less than; Containing diester-type alkaloids with mesaconitine (C
33h
43nO
10), hypaconitine (C
32h
45nO
10) and aconitine (C
33h
43nO
11) total amount, must not 0.020% be crossed.It contains calcium ion not higher than 0.5%w/w, and magnesium ion is not higher than 0.2%w/w, and chloride ion is not higher than 0.5%w/w.It contains calcium ion 0.01% ~ 0.5%w/w, magnesium ion 0.01% ~ 0.2%w/w, chloride ion 0.01% ~ 0.5%w/w.
The concocting method of Radix Aconiti Lateralis Preparata of the present invention or Radix Aconiti Lateralis Preparata, without immersion, its alkaloid of the Radix Aconiti Lateralis Preparata of normal temperature and pressure process also meet 2010 version " Chinese Pharmacopoeia " regulation.Adopt concocting method provided by the invention to prepare without gallbladder Radix Aconiti Lateralis Preparata or Radix Aconiti Lateralis Preparata, owing to not adding edible gallbladder bar in concocting process, so processed product and traditional Radix Aconiti Lateralis Preparata, Radix Aconiti Lateralis Preparata is compared and is greatly reduced wherein calcium ion, magnesium ion, the concentration of chloride ion and other metal ions, reduce toxic and side effects, simultaneously will without gallbladder Radix Aconiti Lateralis Preparata, Radix Aconiti Lateralis Preparata detects by quality standard under " Chinese Pharmacopoeia " version Radix Aconiti Lateralis Preparata item in 2010 respectively, indices all can reach pharmacopoeial requirements, show not add in concocting process edible gallbladder bar without gallbladder Radix Aconiti Lateralis Preparata, Radix Aconiti Lateralis Preparata can reach and Radix Aconiti Lateralis Preparata, the effect that Radix Aconiti Lateralis Preparata is identical.In addition, the present invention has also carried out Inspect and control, for the quality and safety controlled without gallbladder Radix Aconiti Lateralis Preparata or Radix Aconiti Lateralis Preparata provides guarantee comprehensively to without gallbladder Radix Aconiti Lateralis Preparata or Radix Aconiti Lateralis Preparata toxic composition diester-type alkaloids, heavy metal and persticide residue.
Accompanying drawing explanation
Fig. 1 is without gallbladder Radix Aconiti Lateralis Preparata medical material figure (wherein, A: without gallbladder Radix Aconiti Lateralis Preparata; B: without gallbladder Radix Aconiti Lateralis Preparata)
Fig. 2 is without gallbladder Radix Aconiti Lateralis Preparata micro-powder figure
Fig. 3 is without gallbladder Radix Aconiti Lateralis Preparata thin layer figure (No. 1 Radix Aconiti Lateralis Preparata bought for traditional market, No. 2-11 is respectively Qu County Radix Aconiti Lateralis Preparata self-control without gallbladder Radix Aconiti Lateralis Preparata, Radix Aconiti Lateralis Preparata, Monkshood self-control is without gallbladder Radix Aconiti Lateralis Preparata, Radix Aconiti Lateralis Preparata, quality assay self-control presses (2010) without gallbladder Radix Aconiti Lateralis Preparata, Radix Aconiti Lateralis Preparata, quality assay self-control is without gallbladder Radix Aconiti Lateralis Preparata, Radix Aconiti Lateralis Preparata (2011), quality assay self-control is without gallbladder Radix Aconiti Lateralis Preparata, Radix Aconiti Lateralis Preparata (pilot scale), and No. 12-14 is respectively benzoyl mesaconitine, benzoyl aconite alkali, benzoylhypaconitine reference substance)
Fig. 4 six kinds of alkaloid canonical plottings
Fig. 5 reference substance collection of illustrative plates (6 peaks are followed successively by benzoyl mesaconitine, benzoyl aconite alkali, benzoylhypaconitine, mesaconitine, aconitine, hypaconitine reference substance peak)
Fig. 6 is without gallbladder Radix Aconiti Lateralis Preparata collection of illustrative plates
Detailed description of the invention
Embodiment 1 the present invention investigates without gallbladder technique
Get fresh mud Radix Aconiti Lateralis Preparata and be about 10kg, clean, moderate heat (keeping boiling) boils about 15min (to the saturating heart).
Well-done Radix Aconiti Lateralis Preparata is evenly divided into two parts, and portion cuts vertical sheet (thick about 0.3-0.5cm), by medical material leaching drift (20-30min) cut, is then evenly divided into 5 deciles (for concocting Radix Aconiti Lateralis Preparata); Vertical sheet (thick about 0.3-0.5cm) is cut in another part of peeling, by medical material leaching drift (20-30min) cut, is then evenly divided into 5 deciles (for concocting Radix Aconiti Lateralis Preparata).
1.1 steaming times, drying means are examined or check
Five deciles of Radix Aconiti Lateralis Preparata, Radix Aconiti Lateralis Preparata steam about 2h, 4h, 6h, 8h, 10h (normal pressure) respectively.Steamed medical material is distinguished even quadrisection again, adopts oven dry, microwave drying, far-infrared ray drying, drying under reduced pressure four kinds of methods to carry out drying respectively.Add up drying time, dried medical material numbered as follows:
Table 1 four kinds of different dry drying methods compare: (except microwave drying, baking temperature is 55 DEG C)
To sum up, by four kinds of method dryings, the sample appearance that microwave and far-infrared ray drying obtain is bad, do not reach standards of pharmacopoeia, dry and drying under reduced pressure to sample appearance substantially meet standards of pharmacopoeia, but drying under reduced pressure is time-consuming, and waste energy, therefore final selection oven dry is without gallbladder Radix Aconiti Lateralis Preparata and without the drying means of gallbladder than Radix Aconiti Lateralis Preparata.
The Radix Aconiti Lateralis Preparata alkaloid that steaming time difference obtains is different, in table 2:
The different steaming time of table 2 is without gallbladder Radix Aconiti Lateralis Preparata and Radix Aconiti Lateralis Preparata alkaloid content determination result
According to the regulation of " Chinese Pharmacopoeia " version in 2010, Radix Aconiti Lateralis Preparata and Radix Aconiti Lateralis Preparata containing diester-type alkaloids with mesaconitine (C
33h
43nO
10), hypaconitine (C
32h
45nO
10) and aconitine (C
33h
43nO
11) total amount, must not 0.020% be crossed., containing Benzoylmesaconine (C
31h
43nO
10), benzoyl aconine (C
32h
45nO
10) and benzoyl hypo-aconine (C
31h
43nO
9) total amount, must not 0.010% be less than.Visible, the sample steaming 8h post-drying meets States Pharmacopoeia specifications.
1.2 baking temperature examinations
Choose fresh mud Radix Aconiti Lateralis Preparata 4kg, clean, moderate heat boils about 15min (keeping boiling), then two deciles are divided into, portion cuts vertical sheet (thick about 0.3-0.5cm), by medical material leaching drift (20-30min) cut, steam about 8h, then by even for steamed medical material quadrisection; Another part of peeling, section (thick about 0.3-0.5cm), by medical material leaching drift (20-30min) cut, even quadrisection after steaming about 8h; Dry at different temperatures respectively.Test result sees the following form:
The different bake out temperature of table 3 is without gallbladder Radix Aconiti Lateralis Preparata outward appearance and alkaloid comparison sheet
In the Radix Aconiti Lateralis Preparata of usual preparation, the content of monoester alkaloid is higher, and the content of diester-type alkaloids is lower, Radix Aconiti Lateralis Preparata the best in quality.From experimental data in table 3, baking temperature 40-70 DEG C more excellent, and the content of the monoester alkaloid of preparation is high, and the content of diester-type alkaloids is low; Wherein, when the optimal temperature of oven dry is 55 DEG C, better quality, compare and obviously shorten 40 DEG C of drying times, drying time is 24h.
To sum up, processing procedure without gallbladder Radix Aconiti Lateralis Preparata is: get fresh mud Radix Aconiti Lateralis Preparata, clean, moderate heat boils about 15min (keeping boiling), cut vertical sheet (0.3-0.5cm), by medical material leaching drift (20-30min) cut, steam about 8h (normal pressure), take out, dry (55 DEG C, 24h).
Without gallbladder Radix Aconiti Lateralis Preparata processing procedure be: get fresh mud Radix Aconiti Lateralis Preparata, clean, moderate heat boils about 15min (keeping boiling), peeling, cut vertical sheet (0.3-0.5cm), by medical material leaching drift (20-30min) cut, steam about 8h (normal pressure), take out, dry (55 DEG C, 24h).
Quality standard research
1.1 character identification
Black in product without gallbladder: to be longitudinal section, wide at the top and narrow at the bottom, long 1.7-5cm, wide 0.9-3cm, thick 0.2-0.5cm.Crust pitchy, tangent plane dark yellow, glossy tool gloss, translucent, and have longitudinal duct bundle.Matter is hard and crisp, section cutin sample.Feeble QI, lightly seasoned.
Without gallbladder Radix Aconiti Lateralis Preparata: anoderm, yellow-white, translucent, matter is hard and crisp.
Radix Aconiti Lateralis Preparata is processed and Radix Aconiti Lateralis Preparata character consistent (see accompanying drawing 1: without gallbladder Radix Aconiti Lateralis Preparata medical material figure) with traditional method
2.2 microscopical identification
Without gallbladder Radix Aconiti Lateralis Preparata and without gallbladder Radix Aconiti Lateralis Preparata powder ash yellow-white, powder has following structure:
1. starch grain is extremely many, the spherical or round polygon of simple grain class, minority Long Circle, diameter 2-20 μm, and omphalion is point-like, crosswise, people's shape; Composite grain is composited by 2-7 grain or more.
2. metaderm fragment is rare, and surface is seen in polygon, and anticlinal wall is uneven to be thickened, and what have charges into lumen in warty, and cell includes brown thing.
3. stone cell is rare, is dispersed in, and diameter is about 53-125 μm, and pit is obvious.
4. bordered pit and reticulate vessel diameter 20-48 μm.Radix Aconiti Lateralis Preparata master is the parenchyma fragment containing gelatinizing starch grain.To process Radix Aconiti Lateralis Preparata microscopic features consistent with traditional method.(accompanying drawing 2)
2.3 TLC distinguish
Traditional method processing Radix Aconiti Lateralis Preparata 1 batch, without gallbladder Radix Aconiti Lateralis Preparata 5 batches, pulverize respectively without gallbladder Radix Aconiti Lateralis Preparata 5 batches, cross No. four sieves:
Get this product powder 5g, add ammonia solution 5ml moistening, add diethyl ether 50ml, supersound process 30 minutes, filters. and filtrate volatilizes, and the residue 0.5ml that adds methylene chloride makes dissolving, as need testing solution.Separately get Benzoylmesaconine reference substance, benzoyl aconine reference substance, benzoyl hypo-aconine reference substance, add isopropyl alcohol one dichloromethane (1: 1) mixed solution and make every 1ml respectively containing the mixed solution of 1mg, product solution (monoester alkaloid) in contrast.Get mesaconitine reference substance, hypaconitine contrast crystalline substance, aconitine reference substance again, add isopropyl alcohol one dichloromethane (1: 1) mixed solution and make every 1ml respectively containing the mixed solution of 1mg, product solution (diester-type alkaloids) in contrast.Test according to thin layer chromatography (annex VIB), draw need testing solution and each 5 ~ 10 μ l of reference substance solution, put respectively on same silica gel g thin-layer plate, with n-hexane-ethyl acetate-methanol (6.4: 3.6: 1) for developing solvent, put in the ammonia saturated with vapor expansion cylinder of 20 minutes, launch, take out, dry, spray with rare bismuth potassium iodide test solution.In test sample chromatograph, Radix Aconiti Lateralis Preparata or Radix Aconiti Lateralis Preparata on the position corresponding to Benzoylmesaconine reference substance, benzoyl aconine reference substance, benzoyl hypo-aconine reference substance chromatograph, the speckle of aobvious same color.To process Radix Aconiti Lateralis Preparata TLC distinguish speckle consistent with traditional method.(accompanying drawing 3)
The assay of 2.4 alkalies and alkaline earths
Test sample: get quality assay processing and be processed with gallbladder Radix Aconiti Lateralis Preparata 1 batch without gallbladder Radix Aconiti Lateralis Preparata 3 batches, quality assay, the totally 7 batches of medical materials carry out calcium, magnesium, chlorine ion content determination compare to soak gallbladder bar (7 days, 30 days) Radix Aconiti Lateralis Preparata 2 batches, Hebei Anguo purchase Radix Aconiti Lateralis Preparata 1 batch.
2.4.1 the assay of calcium, magnesium ion
Chengdu Branch of the Chinese Academy of Sciences is entrusted to carry out the assay of calcium, magnesium ion.
Detection method: inductively coupled plasma emission spectrography (ICP-AES).
Testing result: in table 4.
2.4.2 the assay of chloride ion
2.4.2.1 Radix Aconiti Lateralis Preparata Radix Aconiti Lateralis Preparata sample (crossing No. four sieves) about 5g is got in the preparation of test sample respectively, and precision takes, and dries to constant weight at 80 DEG C.Separately take food with gallbladder bar appropriate, dry to constant weight equally.Add water 50ml, and supersound process (250W, 50KHz) 30min, lets cool, and supplies weight, shakes up, and filters.Separately get applicable gallbladder bar appropriate, dry to constant weight, use same method process.
2.4.2.2 experimental technique
Accurately pipette test liquid 5ml, gallbladder bar solution 1ml respectively, be placed in 250ml conical flask, add 6ml distilled water, 1ml Neutral potassium chromate indicator, till being titrated to occurring that brick-red precipitation do not disappear with 0.1mol/L silver nitrate standard solution, the silver nitrate solution volume that record consumes.Measurement result is as shown in table 4.
Table 47 batch Radix Aconiti Lateralis Preparata gallbladder bar assay result
Measurement result surface, F
1~ F
3in (without gallbladder Radix Aconiti Lateralis Preparata), the content of calcium, magnesium, chlorine is several times lower than even tens times without the content in gallbladder Radix Aconiti Lateralis Preparata than without gallbladder Radix Aconiti Lateralis Preparata than what soak through gallbladder bar, greatly ensure that the safety of clinical application.Fix tentatively and contain calcium ion not higher than 0.5%w/w without gallbladder Radix Aconiti Lateralis Preparata, magnesium ion is not higher than 0.2%w/w, and chloride ion is not higher than 0.5%w/w.
2.5 heavy metals and harmful element
Test sample: the processing of random selecting quality assay is without gallbladder Radix Aconiti Lateralis Preparata 3 batches, Monkshood processing without gallbladder Radix Aconiti Lateralis Preparata 1 batch, and Qu County processes without gallbladder Radix Aconiti Lateralis Preparata 1 batch, totally 5 batches.
Measure according to lead, cadmium, arsenic, hydrargyrum, copper algoscopy (annex IX B atomic absorption spectrophotometry or inductively coupled plasma mass spectrometry), measurement result is as shown in table 5.
2.5.1 instrument and reagent
U.S. Agilent ICP-MS7500 Inductively coupled plasma mass spectrometry, Shimadzu 100,000/electronics sky
Flat, programmable control temperature microwave counteract appearance (MARS5 type, U.S. CE M company), Millipore Milli-Q ultrapure water system.Nitric acid (external import).
2.5.2 the preparation of standard solution
Plumbous single element standard solution: MERCK, Lot:HC813220 standard value: 1000 ± 2mg/L
Arsenic single element standard solution: MERCK, Lot:HC888556 standard value: 998 ± 5mg/L
Hydrargyrum single element standard solution: MERCK, Lot:HC810358 standard value: 1000 ± 2mg/L
Cadmium single element standard solution: MERCK, Lot:HC813220 standard value: 1000 ± 2mg/L
Copper single element standard solution: MERCK, Lot:HC781459 standard value: 1001 ± 2mg/L
Precision measures above-mentioned lead, arsenic, hydrargyrum, each 200 μ l of cadmium single element standard solution put in 100mL volumetric flask, is settled to scale, shakes up, as stocking standard solution (arsenic, lead, cadmium 2000 μ g/L) with 5% nitric acid; Precision measures above-mentioned copper single element standard solution 1mL and puts in 100mL volumetric flask, is settled to scale, shakes up with 5% nitric acid, as stocking standard solution (copper 10000 μ g/L); Measure above-mentioned standard solution of stocking respectively appropriate, be diluted to each series concentration with 5% nitric acid, be prepared into hybrid standard serial solution.
2.5.3 instrument condition
Radio-frequency power is 1350W, sampling depth 143step, flow rate of carrier gas 0.91L/min, assisted gas flow 0.8L/min, cold gas flow velocity 13L/min, rotating speed 30r/min during peristaltic pump collected specimens, 40 seconds times of integration, repeats 3 times.
2.5.4 the preparation of need testing solution
Get Radix Aconiti Lateralis Preparata powder and be about 0.5g, accurately weighed, put in politef micro-wave diminishing pot, add 7mL nitric acid, place after about 2 hours, setting micro-wave digestion program (power 1600W, per minutely 120 DEG C are warming up to 20 DEG C, keep 5 minutes, per minutely 160 DEG C are warming up to again with 8 DEG C, keep 10 minutes, per minutely 185 DEG C are warming up to again with 5 DEG C, keep 25 minutes), clear up after being cooled to room temperature completely, open interior plug, fling to dense smoke, with deionized water transfer digestion solution in 25mL volumetric flask, and be settled to scale with deionized water, shake up, as need testing solution.Simultaneously with legal system for full reagent sample blank solution.
2.5.5 sample determination
Mark in 75As, 65Cu, 111Cd, 82Se do with 115In (concentration is about 10ppb), 202Hg, 208Pb, with Bi209 (concentration is about 10ppb) do in mark, under above-mentioned instrument condition, above-mentioned standard serial solution is analyzed by peristaltic pump sample introduction, with concentration of element (ppb) for abscissa, corresponding instrument response (ICPS) is vertical coordinate, drawing standard curve; Need testing solution is sample introduction analysis under similarity condition, and bales catch, except after the full reagent blank of sample, reads the concentration (ppb) of each element in need testing solution, and calculates the content of each element in sample from standard curve.Formula is as follows:
Concentration (mg/kg) * 25/ sampling amount/1000 of content (the mg/kg)=need testing solution of each element in sample, measurement result is in table 5.
2.6 Residual Levels of Organochlorine Pesticides
2.6.1 chromatographic condition
Chromatograph: Agilent 6890N gas chromatograph, 63Ni-ECD electron capture detector; Chromatographic column: DB-130m × 0.32mm × 1 μm; Column temperature 70 DEG C (1min), 180 DEG C, 205 DEG C (10min), 280 DEG C of (10min) INJ:250 DEG C; DET:310 DEG C; Nitrogen flow rate: 1.7mL/min; Tail blows: 50mL/min.
2.6.2 the preparation of reference substance solution
Gamma Hexaochlorocyclohexane (total BHC) respectively precision measures 1mL α-BHC reference substance (in the research of national standard material GBW (E) 060081), 1mL β-BHC reference substance (State Standard Matter Research Centre GBW (E) 060082), 1mL γ-BHC reference substance (State Standard Matter Research Centre GBW (E) 060083), 1mL δ-BHC reference substance (State Standard Matter Research Centre GBW (E) 060084) is put in 25mL measuring bottle, dissolve with petroleum ether (60 ~ 90 DEG C) and be diluted to scale, shake up, to obtain final product.
Clofenotane (total DDT) respectively precision measures:
1mLPP '-DDE reference substance (State Standard Matter Research Centre GBW (E) 060104),
1mLPP '-DDD reference substance (State Standard Matter Research Centre GBW (E) 060105),
1mLOP '-DDT reference substance (State Standard Matter Research Centre GBW (E) 060103),
1mLPP '-DDT reference substance (State Standard Matter Research Centre GBW (E) 060102), puts in 25mL measuring bottle, dissolves and is diluted to scale, shake up, to obtain final product with petroleum ether (60 ~ 90 DEG C).
Pentachloronitrobenzene (PCNB) precision measures 1mL pentachloronitrobenzene reference substance (State Standard Matter Research Centre 50 μ g/mL) and puts in 25mL measuring bottle, dissolves and is diluted to scale, shake up, to obtain final product with petroleum ether (60 ~ 90 DEG C).
2.6.3 the preparation of reference substance solution is mixed
Precision measures above-mentioned standard reserving solution α-BHC, γ-BHC, the each 5mL of δ-BHC, the each 10mL of β-BHC, pentachloronitrobenzene (PCNB) 5mL, PP '-DDE, the each 5mL of PP '-DDD, OP '-DDT, the each 10mL of PP '-DDT, put in 100mL measuring bottle, scale is diluted to petroleum ether (60 ~ 90 DEG C), shake up, obtain (α-BHC, γ-BHC, δ-BHC concentration 100ng/mL, β-BHC concentration 200ng/mL, pentachloronitrobenzene (PCNB) concentration 100ng/mL, PP '-DDE, PP '-DDD concentration 100ng/mL, OP '-DDT, PP '-DDT concentration 200ng/mL).
2.6.4 the preparation of need testing solution
Get without gallbladder Radix Aconiti Lateralis Preparata or Radix Aconiti Lateralis Preparata in 60 DEG C of dryings 4 hours, be ground into fine powder, get about 2g, accurately weighed, put in 100mL tool plug conical flask, add water 20mL soaked overnight, precision adds acetone 40mL, weighed weight, supersound process 30 minutes, let cool, weighed weight again, the weight of less loss is supplied with acetone, add sodium chloride again and be about 6g, precision adds dichloromethane 30mL, weighed weight, supersound process 15min, weighed weight again, the weight of less loss is supplied with dichloromethane, leave standstill and make layering, organic facies is moved into rapidly and is equipped with in the 100mL tool plug conical flask of appropriate anhydrous sodium sulfate, place 4h.Precision measures 35mL, be evaporated near dry in 40 DEG C of water-baths, add a small amount of petroleum ether (60 ~ 90 DEG C) if front repeatable operation is to dichloromethane and acetone Ex-all, dissolve with petroleum ether (60 ~ 90 DEG C) and be transferred in 10mL tool plug graduated centrifuge tube, adding petroleum ether (60 ~ 90 DEG C) to 5mL.Carefully add people's sulphuric acid 1mL, jolting 1min, centrifugal 10min, precision measures supernatant 2mL, to obtain final product.
2.6.5 assay method and result
The accurate each 1 μ l of mixing reference substance solution drawing need testing solution and correspond concentration respectively, continuous sample introduction 3 times, gets 3 meansigma methodss respectively, calculates Residual Levels of Organochlorine Pesticides in test sample by external standard method.Result: 5 batches of Radix Aconiti Lateralis Preparata samples all do not detect that organochlorine pesticide (Gamma Hexaochlorocyclohexane, clofenotane, pentachloronitrobenzene) remains.
The Radix Aconiti Lateralis Preparata processing of table 5 main product ground is without gallbladder Radix Aconiti Lateralis Preparata heavy metal and pesticide residue determination
From table 5 by, heavy metal and harmful element measurement result all meet " Chinese Pharmacopoeia " version one in 2010 and must specify: lead must not cross 5/1000000ths; Cadmium must not cross 3/10000000ths; Arsenic must not cross 2/1000000ths, and hydrargyrum must not cross 2/10000000ths, and copper must not cross 20/1000000ths.
Residual Levels of Organochlorine Pesticides all meets " Chinese Pharmacopoeia " version one in 2010 according to pesticide residues quantitative determination and must specify: Gamma Hexaochlorocyclohexane (total BHC) must not cross 2/10000000ths; Clofenotane (total DDT) must not cross 2/10000000ths; Pentachloronitrobenzene (PCNB) must not cross 1/10000000th.
2.7 alkaloidal assays
Test sample: quality assay processing is without gallbladder Radix Aconiti Lateralis Preparata, each 3 batches of Radix Aconiti Lateralis Preparata, Monkshood processing without each 1 batch of gallbladder Radix Aconiti Lateralis Preparata, Radix Aconiti Lateralis Preparata, and Qu County Radix Aconiti Lateralis Preparata is processed without each 1 batch of gallbladder Radix Aconiti Lateralis Preparata, Radix Aconiti Lateralis Preparata, totally 10 batches.
2.7.1 instrument and reagent
Agilent 1200 highly effective liquid phase chromatographic system: comprise 1200 pumps, DAD detector, Millipore Milli-Q ultrapure water system, Shimadzu 100,000/electronic balance, Brasson ultrasonic washing instrument, KQ-100 ultrasonic washing instrument, aconitine (lot number: 110797-200404), mesaconitine (lot number: 110799-200404), hypaconitine (lot number: 110798-200404) reference substance (Nat'l Pharmaceutical & Biological Products Control Institute provides); Benzoyl mesaconitine, benzoylhypaconitine, benzoyl aconite alkali (being provided by new Flos Nelumbinis decoction pieces factory, temporarily without lot number).HPLC methanol, acetonitrile are import chromatographically pure reagent, and all the other are domestic analytical reagent, and HPLC water used is ultra-pure water, and all the other water used are purified water.
2.7.2 chromatographic condition and system suitability
Take octadecylsilane chemically bonded silica as filler, column temperature 20 DEG C; Mobile phase is the biphase gradient elution of A and B, A: acetonitrile, B:40mmol/L ammonium acetate buffer (ammonia adjusts pH=10.0), and according to the form below carries out gradient elution, flow velocity 1ml/min; Determined wavelength is 230nm.Number of theoretical plate calculates should be not less than 3000 by mesaconitine peak.
2.7.3 need testing solution preparation: what precision took 60 mesh sieves is about 2g without gallbladder Radix Aconiti Lateralis Preparata fine powder, and parallel title 3 parts, is placed in 200mL triangular flask respectively, respectively adds 25% ammonia 2mL, moistening 30min.Precision measures extractant isopropyl alcohol-ethyl acetate (1: 1) mixed liquor 100mL, to add in the triangular flask containing sample and weighed weight.After ultrasonic 30min, this sample bottle is placed to room temperature, then weighs, supply the weight lost with extractant, filter after mixing.Precision measures subsequent filtrate 40mL, is concentrated into small size, then it is transferred to evaporate to dryness on an evaporating dish completely with extractant.Residue dissolves also standardize solution with 0.01% hydrochloric acid-methanol and, in 2mL measuring bottle, shakes up, and 0.45 μm of microporous filter membrane filters, and obtains need testing solution.
2.7.4 reference substance solution preparation: precision take mesaconitine, hypaconitine, aconitine reference substance 2.6,1.3,5.19mg puts in same 10mL measuring bottle, dissolve with 0.01% methanol hydrochloride solution and be settled to scale, shake up, obtain diester-type alkaloids reference substance liquid.Precision take benzoyl aconine, benzoyl hypo-aconine, Benzoylmesaconine 4.0256,2.56,1.8mg is respectively placed in 1mL measuring bottle, dissolve with 0.01% methanol hydrochloride solution and be settled to scale, shake up, obtain the reference substance solution of 3 monoester alkaloids.
2.7.5 standard curve preparation: accurately respectively draw appropriate monoester type and diester-type reference substance mixed liquor in same 10ml volumetric flask and add 0.01% hydrochloric acid methanol and be diluted to scale.Then the mixing reference substance solution that appropriate intermediate liquid makes 5 variable concentrations is drawn respectively, analyze by above-mentioned chromatographic condition, carry out regression Calculation (making standard curve with Content of Aconitine and peak area) with peak area (Y) to sample size (X), regression equation is shown in Fig. 4
2.7.6 average recovery test: precision takes Radix Aconiti Lateralis Preparata raw medicinal herbs fine powder 1g totally 30 parts, every 5 parts for a kind of alkaloidal determination of recovery rates, totally 6 groups.It is appropriate that each group sample adds same reference substance solution respectively, carries out preparation and the HPLC analysis of need testing solution by method under need testing solution preparation.Its response rate is calculated according to measured amount and addition.The mean sample recovery rate (RSD) of aconitine, hypaconitine, mesaconitine, benzoyl aconine, benzoyl hypo-aconine, Benzoylmesaconine is respectively 98.70%, 100.47%, 98.20%, 100.35%, 100.27% and 98.47%.
2.7.7 sample determination: precision takes each sample and is about 2g, each sample parallel claims 3 parts, standby by legal system below need testing solution preparation, and carries out the analysis of 3 kinds of monoester alkaloids by above-mentioned chromatographic condition, calculate with accompanying need testing solution on the same day, the results are shown in Table 6.Reference substance and see accompanying drawing 5, Fig. 6 without gallbladder Radix Aconiti Lateralis Preparata HPLC spectrogram.
Table 6 is made by oneself without gallbladder Radix Aconiti Lateralis Preparata assay
According to the regulation of " Chinese Pharmacopoeia " version in 2010, Radix Aconiti Lateralis Preparata and Radix Aconiti Lateralis Preparata monoester alkaloid are with Benzoylmesaconine (C
31h
43nO
10), benzoyl aconine (C
32h
45nO
10) and benzoyl hypo-aconine (C
31h
43nO
9) total amount, must not 0.010% be less than; Containing diester-type alkaloids with mesaconitine (C
33h
43nO
10), hypaconitine (C
32h
45nO
10) and aconitine (C
33h
43nO
11) total amount, must not 0.020% be crossed.
Visible, all batches all meet " Chinese Pharmacopoeia " version in 2010 regulation without gallbladder Radix Aconiti Lateralis Preparata and without gallbladder Radix Aconiti Lateralis Preparata alkaloid.
In sum, adopt concocting method provided by the invention to prepare without gallbladder Radix Aconiti Lateralis Preparata or Radix Aconiti Lateralis Preparata, owing to not adding edible gallbladder bar in concocting process, greatly reduce wherein calcium ion, magnesium ion, the concentration of chloride ion and other metal ions, reduce toxic and side effects, simultaneously will without gallbladder Radix Aconiti Lateralis Preparata, Radix Aconiti Lateralis Preparata detects by quality standard under " Chinese Pharmacopoeia " version Radix Aconiti Lateralis Preparata item in 2010 respectively, indices all can reach pharmacopoeial requirements, show not add in concocting process edible gallbladder bar without gallbladder Radix Aconiti Lateralis Preparata, Radix Aconiti Lateralis Preparata can reach and Radix Aconiti Lateralis Preparata, the effect that Radix Aconiti Lateralis Preparata is identical.And operation in addition, the present invention has also carried out Inspect and control, for the quality and safety controlled without gallbladder Radix Aconiti Lateralis Preparata or Radix Aconiti Lateralis Preparata provides guarantee comprehensively to without gallbladder Radix Aconiti Lateralis Preparata or Radix Aconiti Lateralis Preparata toxic composition diester-type alkaloids, heavy metal and persticide residue.
Claims (3)
1. without a concocting method for gallbladder Radix Aconiti Lateralis Preparata, it is characterized in that: it is concocted according to the following steps:
A, get fresh mud Radix Aconiti Lateralis Preparata, clean; Moderate heat keeps boiling to boil 10-20min;
B, section, leaching drift 20-30min, 105 DEG C of-110 DEG C of temperature, normal pressure steams 8h;
C, drying, to obtain final product; Described drying means is 55 DEG C dries 24h.
2. concocting method according to claim 1, is characterized in that: in described concocting method, a step is peelled off crust, cut vertical sheet after boiling, and thickness is 0.3cm-0.5cm.
3. concocting method according to claim 1, is characterized in that: in described concocting method a step boil after not peeling, cut vertical sheet, thickness is 0.3cm-0.5cm.
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| CN105213516B (en) * | 2015-11-05 | 2019-03-08 | 西南科技大学 | A kind of no gallbladder radix aconiti lateralis preparata concocting method |
| CN105784914A (en) * | 2016-04-18 | 2016-07-20 | 山东明人福瑞达卫生材料有限公司 | Detection method for traditional Chinese medicine muskiness strong bone plasters |
| CN107184672A (en) * | 2017-06-24 | 2017-09-22 | 河南省青山药业有限公司 | A kind of black preparation method along piece |
| CN108904654A (en) * | 2018-08-15 | 2018-11-30 | 康美滕王阁（四川）制药有限公司 | A kind of rhizoma typhonii processing procedure and products thereof |
| CN108904609A (en) * | 2018-08-15 | 2018-11-30 | 康美滕王阁（四川）制药有限公司 | A kind of RADIX ACONITILATERALIS PREPARATA processing procedure and products thereof and application |
| CN109045122A (en) * | 2018-08-15 | 2018-12-21 | 康美滕王阁（四川）制药有限公司 | Black suitable piece processing procedure of one kind and products thereof and application |
| CN112051351A (en) * | 2020-08-28 | 2020-12-08 | 康美药业股份有限公司 | Thin-layer chromatography identification method for Heishui tablets |
| CN116637139A (en) * | 2023-06-26 | 2023-08-25 | 城固县群利中药材专业合作社 | Dry accessory slices for fixation and preparation method thereof, black accessory slices and preparation method thereof |
| CN116870057A (en) * | 2023-06-26 | 2023-10-13 | 陕西师范大学 | Dried aconite root and dried aconite root tablet and its preparation method |
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