CN102429966A - Gall-free Heishunpian or rhizoma typhonii tablet and processing method thereof - Google Patents
Gall-free Heishunpian or rhizoma typhonii tablet and processing method thereof Download PDFInfo
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Abstract
The invention provides a processing method of gall-free Heishunpian or rhizoma typhonii tablet. The processing method comprises the following steps of: a. cleaning fresh rhizoma typhonii, and boiling a little at medium fire for 10-20 minutes; b. slicing, soaking and rinsing for 20-30 minutes, and steaming at the temperature of 105-110 DEG C under normal pressure for 2-10 hours; and c. drying. The invention also provides the gall-free Heishunpian or rhizoma typhonii tablet prepared by the processing method, and edible dried gall is not added in the processing process. By adopting the processing method provided by the invention, the contents of calcium ion, magnesium ion, chloride ion and other metal ions in the processed product are greatly reduced, the clinical efficacy is guaranteed, the toxic or side effect is reduced and the medicine safety is improved.
Description
Technical field
The present invention relates to a kind of no 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, and it is supporing yang to mend fire, the effect of dispersing cold for relieving pain; Be used for the YANG-depletion collapse, cold extremities faint pulse, sexual impotence cold womb; Coldness and pain in the epigastrium, deficiency and coldness is vomited and diarrhoea, the YIN-cold edema; The 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 family particularly payes attention on its processing procedure method in order to subtract its toxicity, to improve clinical efficacy at all times.Radix Aconiti Lateralis Preparata is as the conventional Chinese medicine material, and Radix Aconiti Lateralis Preparata or Radix Aconiti Lateralis Preparata are that its decoction pieces is in one of the most common specification of clinical practice.
Traditional concocting method of Radix Aconiti Lateralis Preparata is: get the mud Radix Aconiti Lateralis Preparata, clean, immerse a few days in the aqueous solution that eats the gallbladder crust, boil to passing through the heart together with immersion; Pull out, water floats, the sheet of rip cutting Cheng Houyue 0.5cm; The reuse water logging is floated, and makes Radix Aconiti Lateralis Preparata dye Umber with toning liquid, takes out; Steam after pasta, gloss occur, baking is to half-dried, dries or continues oven dry.Radix Aconiti Lateralis Preparata through the heat treated of steaming and decocting, makes its toxic component diester-type alkaloids hydrolysis become the less monoester alkaloid of toxicity after water floats, and has both destroyed toxic component, does not influence its heart tonifying composition again, has guaranteed clinical efficacy when having reached Attenuation.[Lu Nan. the simple analysis of Radix Aconiti Lateralis Preparata processing procedure method. " practical tcm internal medicine journal .2010,24:98-100]
Traditional concocting method of Radix Aconiti Lateralis Preparata is: select mud Radix Aconiti Lateralis Preparata of uniform size, clean, immerse a few days in the aqueous solution that eats the gallbladder crust, boil to passing through the 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 and pass through, dry, practise and claim " Radix Aconiti Lateralis Preparata ".
But modern study proves; Used gallbladder crust contains a large amount of calcium ions, magnesium ion, chloride ion and other metal ions in the Radix Aconiti Lateralis Preparata or the Radix Aconiti Lateralis Preparata course of processing, and the content of calcium, magnesium, chloride ion approximately is respectively in present traditional concocting method: 1.7%, 0.3%, 3.8%.Calcium, magnesium ion have intensive corrosiveness to stomach, make the protein coagulating of human organ, and magnesium ion can suppress cardiovascular and nervous system after being absorbed, and the people is had bigger toxicity.Though the mud Radix Aconiti Lateralis Preparata wants flowing water to take off gallbladder 5～6 times after the immersion of gallbladder crust, it is complete also can not to take off gallbladder, and the lawless person is more arranged, and in Radix Aconiti Lateralis Preparata, pours into the gallbladder crust in a large number and makes the Radix Aconiti Lateralis Preparata weightening finish.Therefore, bigger by the Radix Aconiti Lateralis Preparata or the Radix Aconiti Lateralis Preparata toxic and side effects of traditional concocting method preparation, in safety, there is certain hidden danger.
Though many in recent years scholars have carried out continuous exploration, employ new technology and improve the processing technique of Radix Aconiti Lateralis Preparata.Adopt even experimental design method like Liu Huiru etc., optimize that best processing procedure be that bright Radix Aconiti Lateralis Preparata adds 0.1% gallbladder crust, decocte with water 3 hours was floated 2 days, steamed 2 hours, and concocted time can shorten 8 days; Hu Sumei etc. adopt saturated aqueous common salt to replace gallbladder crust liquid to concoct Radix Aconiti Lateralis Preparata, and this author thinks that Radix Aconiti Lateralis Preparata must pass through long-time immersion and could reduce its toxicity; The method for preparing complex process, high to the requirement of equipment, and also these processing technique all do not have the checking through excessive production, can not satisfy big production demand.
Summary of the invention
Technical scheme of the present invention has provided a kind of concocting method of not having gallbladder Radix Aconiti Lateralis Preparata or Radix Aconiti Lateralis Preparata, and it does not add the gallbladder crust in concocting process.Another technical scheme of the present invention has provided the no gallbladder Radix Aconiti Lateralis Preparata or the Radix Aconiti Lateralis Preparata of this concocting method preparation.
The invention provides a kind of concocting method of not having gallbladder Radix Aconiti Lateralis Preparata or Radix Aconiti Lateralis Preparata, it may further comprise the steps:
A, get fresh mud Radix Aconiti Lateralis Preparata, clean; Moderate heat keeps boiling to boil 10-20min;
B, section are soaked and are floated 20-30min, float to slice surface inviscidly, and 105 ℃ of-110 ℃ of temperature, normal pressure steams 2-10h;
C, oven dry promptly get.
Wherein, the described steaming time of b step is 8h.
Wherein, the described drying means of c step is 40 ℃-70 ℃ oven dry 17h-73h.
Wherein, the described drying means of c step is 55 ℃ of oven dry 24h.
Wherein, the concocting method of described no gallbladder Radix Aconiti Lateralis Preparata is: peelling off crust after boiling, cutting vertical sheet thickness is 0.3cm-0.5cm.
Wherein, the concocting method of described no gallbladder Radix Aconiti Lateralis Preparata is: not peeling after boiling, cut vertical sheet, thickness is 0.3cm-0.5cm.
The present invention also provides the no gallbladder Radix Aconiti Lateralis Preparata or the Radix Aconiti Lateralis Preparata of described concocting method preparation.
It contains monoester alkaloid with Benzoylmesaconine (C
31H
43NO
10), benzoyl aconine (C
32H
45NO
10) and benzoyl hypo-aconine (C
31H
43NO
9) the total amount meter, must not be less than 0.010%; Contain diester-type alkaloids with mesaconitine (C
33H
43NO
10), hypaconitine (C
32H
45NO
10) and aconitine (C
33H
43NO
11) the total amount meter, must not cross 0.020%.It contains calcium ion and is 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 Radix Aconiti Lateralis Preparata that normal temperature and pressure is handled also meets the version " regulation of Chinese pharmacopoeia in 2010.Adopt the no gallbladder Radix Aconiti Lateralis Preparata or the Radix Aconiti Lateralis Preparata of concocting method preparation provided by the invention; Owing in concocting process, do not add edible gallbladder crust; So comparing with traditional Radix Aconiti Lateralis Preparata, Radix Aconiti Lateralis Preparata, processed product greatly reduces the wherein concentration of calcium ion, magnesium ion, chloride ion and other metal ions; Reduced toxic and side effects; To there be gallbladder Radix Aconiti Lateralis Preparata, Radix Aconiti Lateralis Preparata simultaneously respectively by " quality standard detects under Chinese pharmacopoeia version Radix Aconiti Lateralis Preparata in 2010 item, and each item index all can reach the pharmacopeia requirement, shows that the no gallbladder Radix Aconiti Lateralis Preparata, the Radix Aconiti Lateralis Preparata that do not add edible gallbladder crust in the concocting process can reach and Radix Aconiti Lateralis Preparata, effect that Radix Aconiti Lateralis Preparata is identical.In addition, the present invention also monitors and controls no gallbladder Radix Aconiti Lateralis Preparata or Radix Aconiti Lateralis Preparata toxic composition diester-type alkaloids, heavy metal and persticide residue, for the quality and safety property of controlling no gallbladder Radix Aconiti Lateralis Preparata or Radix Aconiti Lateralis Preparata provides assurance comprehensively.
Description of drawings
Fig. 1 does not have gallbladder Radix Aconiti Lateralis Preparata medical material figure (wherein, A: no gallbladder Radix Aconiti Lateralis Preparata; B: no gallbladder Radix Aconiti Lateralis Preparata)
Fig. 2 does not have gallbladder Radix Aconiti Lateralis Preparata powder microgram
Fig. 3 does not have gallbladder Radix Aconiti Lateralis Preparata thin layer figure (No. 1 Radix Aconiti Lateralis Preparata for the traditional market purchase; Be respectively the no gallbladder Radix Aconiti Lateralis Preparata of Qu County Radix Aconiti Lateralis Preparata self-control, Radix Aconiti Lateralis Preparata for 2-11 number; The no gallbladder Radix Aconiti Lateralis Preparata of Butuo Radix Aconiti Lateralis Preparata self-control, Radix Aconiti Lateralis Preparata, the no gallbladder Radix Aconiti Lateralis Preparata of river oil Radix Aconiti Lateralis Preparata self-control, Radix Aconiti Lateralis Preparata are pressed (2010), the no gallbladder Radix Aconiti Lateralis Preparata of river oil Radix Aconiti Lateralis Preparata self-control, Radix Aconiti Lateralis Preparata (2011); The no gallbladder Radix Aconiti Lateralis Preparata of river oil Radix Aconiti Lateralis Preparata self-control, Radix Aconiti Lateralis Preparata (pilot scale) are respectively benzoyl mesaconitine, benzoyl aconite alkali, benzoylhypaconitine reference substance 12-14 number)
Six kinds of alkaloid canonical plottings of Fig. 4
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 does not have gallbladder Radix Aconiti Lateralis Preparata collection of illustrative plates
The specific embodiment
Embodiment 1 the present invention does not have gallbladder technology and investigates
Get the fresh about 10kg of mud Radix Aconiti Lateralis Preparata, clean, moderate heat (keeping boiling) boils about 15min (to passing through the heart).
Well-done Radix Aconiti Lateralis Preparata evenly is divided into two parts, and portion is cut vertical sheet (thick about 0.3-0.5cm), the medical material that cuts is soaked float (20-30min), evenly is divided into 5 five equilibriums (being used to concoct Radix Aconiti Lateralis Preparata) then; Vertical sheet (thick about 0.3-0.5cm) is cut in another part peeling, the medical material that cuts is soaked float (20-30min), evenly is divided into 5 five equilibriums (being used to concoct Radix Aconiti Lateralis Preparata) then.
1.1 steaming time, drying means examination
Five five equilibriums of Radix Aconiti Lateralis Preparata, Radix Aconiti Lateralis Preparata steam about 2h, 4h, 6h, 8h, 10h (normal pressure) respectively.Distinguish even quadrisection again with steaming good medical material, adopt oven dry, microwave drying, far-infrared ray drying, four kinds of methods of drying under reduced pressure to carry out drying respectively.Add up drying time, the medical material that drying is good is numbered as follows:
Four kinds of different dry drying methods of table 1 compare: (except that microwave drying, baking temperature is 55 ℃)
To sum up; Through four kinds of method dryings, the sample appearance that microwave and far-infrared ray drying obtain is bad, does not reach standards of pharmacopoeia; The oven dry and drying under reduced pressure to sample appearance meet standards of pharmacopoeia basically; But drying under reduced pressure is time-consuming, and wastes energy, so final selection oven dry is no gallbladder Radix Aconiti Lateralis Preparata and does not have the drying means of gallbladder than Radix Aconiti Lateralis Preparata.
The Radix Aconiti Lateralis Preparata alkaloid that the steaming time difference obtains is different, sees table 2:
The different steaming times of table 2 do not have gallbladder Radix Aconiti Lateralis Preparata and Radix Aconiti Lateralis Preparata alkaloid content determination result
According to " regulation that Chinese pharmacopoeia version in 2010 is an one, Radix Aconiti Lateralis Preparata and Radix Aconiti Lateralis Preparata contain diester-type alkaloids with mesaconitine (C
33H
43NO
10), hypaconitine (C
32H
45NO
10) and aconitine (C
33H
43NO
11) the total amount meter, must not cross 0.020%., contain Benzoylmesaconine (C
31H
43NO
10), benzoyl aconine (C
32H
45NO
10) and benzoyl hypo-aconine (C
31H
43NO
9) total amount, must not be less than 0.010%.Thus it is clear that, steam the sample of drying behind the 8h and meet the pharmacopeia regulation.
1.2 baking temperature examination
Choose fresh mud Radix Aconiti Lateralis Preparata 4kg, clean, moderate heat boils about 15min (keeping boiling), is divided into two five equilibriums then, and portion is cut vertical sheet (thick about 0.3-0.5cm), the medical material that cuts is soaked float (20-30min), steams about 8h, will steam the good even quadrisection of medical material then; Another part peeling, section (thick about 0.3-0.5cm) is soaked the medical material that cuts and is floated (20-30min), steams even quadrisection behind about 8h; Under different temperatures, dry respectively.Test result sees the following form:
The different bake out temperatures of table 3 do not have gallbladder Radix Aconiti Lateralis Preparata outward appearance and alkaloid comparison sheet
Usually the content of monoester alkaloid is high more in the Radix Aconiti Lateralis Preparata of preparation, and the content of diester-type alkaloids is low more, Radix Aconiti Lateralis Preparata the best in quality.Can be known that by experimental data in the table 3 baking temperature 40-70 ℃ more excellent, 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 was 55 ℃, better quality was compared and is obviously shortened 40 ℃ of drying times, and be 24h drying time.
To sum up, the processing procedure of no gallbladder Radix Aconiti Lateralis Preparata is: get fresh mud Radix Aconiti Lateralis Preparata, clean, moderate heat boils about 15min (keeping boiling), cuts vertical sheet (0.3-0.5cm), the medical material that cuts is soaked float (20-30min), steams about 8h (normal pressure), take out, oven dry (55 ℃, 24h).
No gallbladder Radix Aconiti Lateralis Preparata processing procedure is: get fresh mud Radix Aconiti Lateralis Preparata, clean, moderate heat boils about 15min (keeping boiling), and vertical sheet (0.3-0.5cm) is cut in peeling, the medical material that cuts is soaked float (20-30min), steams about 8h (normal pressure), take out, oven dry (55 ℃, 24h).
Quality standard research
1.1 character identification
No gallbladder is black in article: be longitudinal section, and wide at the top and narrow at the bottom, long 1.7-5cm, wide 0.9-3cm, thick 0.2-0.5cm.The crust pitchy, the tangent plane dark yellow, glossy tool gloss, translucent, and the longitudinal duct bundle is arranged.Matter is hard and crisp, section cutin appearance.Feeble QI, lightly seasoned.
No gallbladder Radix Aconiti Lateralis Preparata: anoderm, yellow-white, translucent, matter is hard and crisp.
Consistently with traditional method processing Radix Aconiti Lateralis Preparata and Radix Aconiti Lateralis Preparata character (see accompanying drawing 1: no gallbladder Radix Aconiti Lateralis Preparata medical material figure)
2.2 microscopical identification
No gallbladder Radix Aconiti Lateralis Preparata and do not have gallbladder Radix Aconiti Lateralis Preparata powder ash yellow-white, powder has following structure:
1. starch grain is extremely many, the spherical or circle polygon of simple grain class, and the minority Long Circle, diameter 2-20 μ m, omphalion is point-like, crosswise, herringbone shape; Composite grain by 2-7 grain or more being composited more.
2. the metaderm fragment is rare, and the surface is seen and is polygon, and anticlinal wall is inhomogeneous to be thickened, and the warty that is that has is charged into lumen, and cell includes brown thing.
3. stone cell is rare, be dispersed in, and the about 53-125 μ of diameter m, pit is obvious.
4. bordered pit and reticulate vessel diameter 20-48 μ m.The Radix Aconiti Lateralis Preparata master is the parenchyma fragment that contains the gelatinizing starch grain.Consistent with traditional method processing Radix Aconiti Lateralis Preparata microscopic features.(accompanying drawing 2)
2.3 thin layer is differentiated
1 batch of traditional method processing Radix Aconiti Lateralis Preparata, 5 batches of no gallbladder Radix Aconiti Lateralis Preparata, 5 batches of pulverize separately of no gallbladder Radix Aconiti Lateralis Preparata, cross sieve No. four:
These article of getting powder 5g adds ammonia solution 5ml moistening, the 50ml that adds diethyl ether, and supersound process 30 minutes filters. and filtrating volatilizes, and the residue 0.5ml that adds methylene chloride makes dissolving, as need testing solution.Other gets Benzoylmesaconine reference substance, benzoyl aconine reference substance, benzoyl hypo-aconine reference substance; Add isopropyl alcohol one dichloromethane (1: 1) mixed solution and process the mixed solution that every 1ml contains 1mg, as reference substance solution (monoester alkaloid).Get mesaconitine reference substance, brilliant, the aconitine reference substance of hypaconitine contrast again, add isopropyl alcohol one dichloromethane (1: 1) mixed solution and process the mixed solution that every 1ml contains 1mg, as reference substance solution (diester-type alkaloids).According to thin layer chromatography (appendix VIB) test, draw each 5～10 μ l of need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate; With normal hexane-ethyl acetate-methanol (6.4: 3.6: 1) is developing solvent; Put in 20 minutes the expansion cylinder of ammonia saturated with vapor, launch, take out; Dry, spray is with rare bismuth potassium iodide test solution.In the test sample chromatograph, Radix Aconiti Lateralis Preparata or Radix Aconiti Lateralis Preparata with Benzoylmesaconine reference substance, benzoyl aconine reference substance, the corresponding position of benzoyl hypo-aconine reference substance chromatograph on, show the speckle of same color.Differentiate that with traditional method processing Radix Aconiti Lateralis Preparata thin layer speckle is consistent.(accompanying drawing 3)
2.4 the assay of alkalies and alkaline earth
Specimen: get 3 batches of no gallbladder Radix Aconiti Lateralis Preparatas of river oil Radix Aconiti Lateralis Preparata processing, river oil Radix Aconiti Lateralis Preparata is processed with 1 batch of gallbladder Radix Aconiti Lateralis Preparata, soak gallbladder crust (7 days, 30 days) 2 batches of Radix Aconiti Lateralis Preparatas, Hebei Anguo buy 1 batch of Radix Aconiti Lateralis Preparata the totally 7 batches of medical materials carry out calcium, magnesium, chlorine ion content determination and compare.
2.4.1 the assay of calcium, magnesium ion
Entrust Chengdu Branch of the Chinese Academy of Sciences to carry out the assay of calcium, magnesium ion.
Detection method: inductively coupled plasma emission spectrography (ICP-AES).
Testing result: see table 4.
2.4.2 the assay of chloride ion
2.4.2.1 the about 5g of Radix Aconiti Lateralis Preparata Radix Aconiti Lateralis Preparata sample (crossing sieve No. four) is got in the preparation of test sample respectively, precision takes by weighing, and under 80 ℃, dries to constant weight.It is an amount of that other gets edible gallbladder crust, dries to constant weight equally.Add water 50ml, supersound process (put coldly, supplies weight, shakes up, and filters by 250W, 50KHz) 30min.Other gets and is suitable for the gallbladder crust in right amount, dries to constant weight, and uses with quadrat method and handles.
2.4.2.2 experimental technique
Accurately pipette test liquid 5ml, gallbladder crust solution 1ml respectively; Place the 250ml conical flask, add the 6ml distilled water, 1ml Neutral potassium chromate indicator; With 0.1mol/L silver nitrate standard solution titration till brick-red deposition occurs and do not disappear, the silver nitrate solution volume that record consumes.Mensuration result is as shown in table 4.
Table 47 crowd Radix Aconiti Lateralis Preparata gallbladder crust assay result
Mensuration result surface, F
1～F
3The content of calcium, magnesium, chlorine is several times lower than even tens times than no gallbladder Radix Aconiti Lateralis Preparata than the content in the no gallbladder Radix Aconiti Lateralis Preparata that soaks through the gallbladder crust in (no gallbladder Radix Aconiti Lateralis Preparata), has guaranteed clinical application safety greatly.Tentative no gallbladder Radix Aconiti Lateralis Preparata contains calcium ion and is 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.
2.5 heavy metal and harmful element
Specimen: 3 batches of no gallbladder Radix Aconiti Lateralis Preparatas of picked at random river oil Radix Aconiti Lateralis Preparata processing, 1 batch of the no gallbladder Radix Aconiti Lateralis Preparata of Butuo Radix Aconiti Lateralis Preparata processing, 1 batch of the no gallbladder Radix Aconiti Lateralis Preparata of Qu County processing, totally 5 batches.
Measure according to lead, cadmium, arsenic, hydrargyrum, copper algoscopy (appendix IX B atomic absorption spectrophotometry or inductively coupled plasma mass spectrometry), it is as shown in table 5 to measure the result.
2.5.1 instrument and reagent
U.S. Agilent ICP-MS7500 inductively coupled plasma mass spectrograph, 100,000/electronics sky, Tianjin, island
Flat, temperature control microwave dissolver able to programme (MARS5 type, U.S. CE M company), Millipore Milli-Q ultra-pure 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 is measured each 200 μ l of above-mentioned lead, arsenic, hydrargyrum, cadmium single element standard solution and is put in the 100mL volumetric flask, is settled to scale with 5% nitric acid, shakes up, as stocking standard solution (arsenic, lead, cadmium 2000 μ g/L); Precision is measured above-mentioned copper single element standard solution 1mL and is put in the 100mL volumetric flask, is settled to scale with 5% nitric acid, shakes up, as stocking standard solution (copper 10000 μ g/L); Measure respectively that above-mentioned to stock standard solution an amount of, be diluted to each series concentration, be prepared into hybrid standard series solution with 5% nitric acid.
2.5.3 instrument condition
Radio-frequency power is 1350W, sampling depth 143step, and flow rate of carrier gas 0.91L/min, secondary air amount 0.8L/min, cold gas flow velocity 13L/min, rotating speed 30r/min during the peristaltic pump collected specimens, repeats 3 times 40 seconds times of integration.
2.5.4 the preparation of need testing solution
Get the about 0.5g of Radix Aconiti Lateralis Preparata powder, the accurate title, decide, and puts in the politef micro-wave digestion jar, adds 7mL nitric acid; After placing about 2 hours, (power 1600W is warming up to 120 ℃ with 20 ℃ of per minutes, keeps 5 minutes to set the micro-wave digestion program; Be warming up to 160 ℃ with 8 ℃ of per minutes again, kept 10 minutes, be warming up to 185 ℃ with 5 ℃ of per minutes again, kept 25 minutes); Clear up be cooled to room temperature fully after, open interior plug, fling to dense smoke, shift digestion solution to the 25mL volumetric flask with deionized water; And be settled to scale with deionized water, shake up, as need testing solution.Simultaneously prepare full reagent sample blank solution with method.
2.5.5 sample determination
Mark in 75As, 65Cu, 111Cd, 82Se do with 115In (the about 10ppb of concentration); 202Hg, 208Pb, do with Bi209 (the about 10ppb of concentration) in mark; Under above-mentioned instrument condition, above-mentioned standard serial solution is analyzed by the peristaltic pump sample introduction; With concentration of element (ppb) is abscissa, and corresponding instrument response (ICPS) is a vertical coordinate, the drawing standard curve; Need testing solution is the sample introduction analysis under similarity condition, and bales catch is read the concentration (ppb) of each element the need testing solution from standard curve, and calculated the content of each element in the sample after removing the full reagent blank of sample.Formula is following:
Concentration (mg/kg) * 25/ sampling amount/1000 of the content of each element (mg/kg)=need testing solution in the sample are measured the result and are seen 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 μ m; 70 ℃ of (1min), 180 ℃, 205 ℃ (10min) of column temperature, 280 ℃ (10min) INJ:250 ℃; DET:310 ℃; Nitrogen flow rate: 1.7mL/min; Tail blows: 50mL/min.
2.6.2 the preparation of reference substance solution
Gamma Hexaochlorocyclohexane (total BHC) precision is respectively measured 1mL α-BHC reference substance (GBW (E) 060081 in the research of national standard material); 1mL β-BHC reference substance (GBW of State Standard Matter Research Centre (E) 060082); 1mL γ-BHC reference substance (GBW of State Standard Matter Research Centre (E) 060083), 1mL δ-BHC reference substance (GBW of State Standard Matter Research Centre (E) 060084) puts in the 25mL measuring bottle, dissolves and is diluted to scale with petroleum ether (60～90 ℃); Shake up, promptly get.
Clofenotane (total DDT) precision is respectively measured:
1mLPP '-DDE reference substance (GBW of State Standard Matter Research Centre (E) 060104),
1mLPP '-DDD reference substance (GBW of State Standard Matter Research Centre (E) 060105),
1mLOP '-DDT reference substance (GBW of State Standard Matter Research Centre (E) 060103),
1mLPP '-DDT reference substance (GBW of State Standard Matter Research Centre (E) 060102) puts in the 25mL measuring bottle, dissolves and is diluted to scale with petroleum ether (60～90 ℃), shakes up, and promptly gets.
Pentachloronitrobenzene (PCNB) precision is measured 1mL pentachloronitrobenzene reference substance (the 50 μ g/mL of State Standard Matter Research Centre) and is put in the 25mL measuring bottle, dissolves and is diluted to scale with petroleum ether (60～90 ℃), shakes up, and promptly gets.
2.6.3 mix the preparation of reference substance solution
Precision is measured above-mentioned standard reserving solution α-BHC, γ-BHC, each 5mL of δ-BHC, each 10mL of β-BHC, pentachloronitrobenzene (PCNB) 5mL, PP '-DDE, each 5mL of PP '-DDD; OP '-DDT, each 10mL of PP '-DDT put in the 100mL measuring bottle, are diluted to scale with petroleum ether (60～90 ℃); Shake up; Promptly get (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 no gallbladder Radix Aconiti Lateralis Preparata or Radix Aconiti Lateralis Preparata in 60 ℃ of dryings 4 hours, be ground into fine powder, get about 2g, accurately claim surely, put in the 100mL tool plug conical flask; Add water 20mL soaked overnight, precision adds acetone 40mL, claims to decide weight, supersound process 30 minutes; Put coldly, claim again to decide weight, supply the weight that subtracts mistake, add the about 6g of sodium chloride again with acetone; The accurate dichloromethane 30mL that adds claims to decide weight, and supersound process 15min claims to decide weight again; Supply the weight that subtracts mistake with dichloromethane, leave standstill and make layering, organic facies is moved into rapidly be equipped with in the 100mL tool plug conical flask of an amount of anhydrous sodium sulfate, place 4h.Precision is measured 35mL; Be evaporated near doing in 40 ℃ of water-baths; Add a small amount of petroleum ether (60～90 ℃) like preceding repeatable operation to dichloromethane and acetone Ex-all, dissolve and be transferred in the 10mL tool plug graduated centrifuge tube, add petroleum ether (60～90 ℃) to 5mL with petroleum ether (60～90 ℃).Carefully add people's sulphuric acid 1mL, jolting 1min, centrifugal 10min, precision is measured supernatant 2mL, promptly gets.
2.6.5 assay method and result
Respectively accurate need testing solution and each 1 μ l of mixing reference substance solution of corresponding concentration with it of drawing, continuous sample introduction is 3 times respectively, gets meansigma methods 3 times, by Residual Levels of Organochlorine Pesticides in the external standard method calculating test sample.The result: it is residual that the 5 batches of Radix Aconiti Lateralis Preparata samples all do not detect organochlorine pesticide (Gamma Hexaochlorocyclohexane, clofenotane, pentachloronitrobenzene).
Table 5 main product ground Radix Aconiti Lateralis Preparata no gallbladder Radix Aconiti Lateralis Preparata heavy metal of processing and pesticide residue determination
By visible, heavy metal and harmful element are measured the result and are met all that " Chinese pharmacopoeia one one of version in 2010 must be stipulated: lead must not cross 5/1000000ths by table 5; 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 meets all according to the pesticide residues quantitative determinations that " Chinese pharmacopoeia one one of version in 2010 must be stipulated: 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 alkaloids content is measured
Specimen: the no gallbladder Radix Aconiti Lateralis Preparata of river oil Radix Aconiti Lateralis Preparata processing, each 3 batches of Radix Aconiti Lateralis Preparatas, Butuo Radix Aconiti Lateralis Preparata are processed each 1 batch of no gallbladder Radix Aconiti Lateralis Preparata, Radix Aconiti Lateralis Preparata, each 1 batch of the no gallbladder Radix Aconiti Lateralis Preparata of Qu County Radix Aconiti Lateralis Preparata processing, Radix Aconiti Lateralis Preparata, totally 10 batches.
2.7.1 instrument and reagent
Agilent 1200 highly effective liquid phase chromatographic systems: comprise 1200 pumps; The DAD detector; Millipore Milli-Q ultra-pure water system, Tianjin, island 100,000/electronic balance, Brasson ultrasonic washing instrument; The 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 (provide by new Flos Nelumbinis decoction pieces factory, do not have lot number temporarily).HPLC is import chromatographically pure reagent with methanol, acetonitrile, and all the other are homemade AR, and HPLC institute water is a ultra-pure water, and all the other institute's waters are purified water.
2.7.2 chromatographic condition and system suitability test
With the octadecylsilane chemically bonded silica is filler, 20 ℃ of column temperatures; Mobile phase is A and the biphase gradient elution of B, A: acetonitrile, and B:40mmol/L ammonium acetate buffer (ammonia is transferred pH=10.0), according to the form below carries out gradient elution, flow velocity 1ml/min; The detection wavelength is 230nm.Number of theoretical plate calculates by the mesaconitine peak should be not less than 3000.
2.7.3 the need testing solution preparation: precision took by weighing the about 2g of no gallbladder Radix Aconiti Lateralis Preparata fine powder of 60 mesh sieves, and 3 parts of parallel titles place the 200mL triangular flask respectively, respectively add 25% ammonia 2mL, moistening 30min.Precision is measured extractant isopropyl alcohol-ethyl acetate (1: 1) mixed liquor 100mL, adds to also to claim to decide weight in the triangular flask that contains sample.Behind the ultrasonic 30min, this sample bottle is placed to room temperature, weighs again, supply the weight that loses, filter behind the mixing with extractant.Precision is measured subsequent filtrate 40mL, is concentrated into small size, again it is transferred to evaporate to dryness on the evaporating dish fully with extractant.Residue, shakes up in the 2mL measuring bottle with 0.01% hydrochloric acid-dissolve with methanol and standardize solution, and 0.45 μ m microporous filter membrane filters, need testing solution.
2.7.4 reference substance solution preparation: precision takes by weighing mesaconitine, hypaconitine, aconitine reference substance 2.6,1.3,5.19mg and puts in the same 10mL measuring bottle; With 0.01% methanol hydrochloride solution dissolving and be settled to scale; Shake up, get diester-type alkaloids reference substance liquid.Precision takes by weighing benzoyl aconine, benzoyl hypo-aconine, Benzoylmesaconine 4.0256,2.56,1.8mg and respectively places in the 1mL measuring bottle; With 0.01% methanol hydrochloride solution dissolving and be settled to scale; Shake up, get the reference substance solution of 3 monoester alkaloids.
2.7.5 standard curve preparation: accurate respectively an amount of monoester type and the diester-type reference substance mixed liquor drawn is in same 10ml volumetric flask and add 0.01% hydrochloric acid methanol and be diluted to scale.Draw an amount of intermediate liquid then respectively and process the mixing reference substance solution of 5 variable concentrations, analyze by above-mentioned chromatographic condition, with peak area (Y) sample size (X) is carried out regression Calculation (making standard curve with aconitine content and peak area), regression equation is seen Fig. 4
2.7.6 the average recovery test: precision takes by weighing totally 30 parts of Radix Aconiti Lateralis Preparata raw medicinal herbs fine powder 1g, and per 5 parts are used for a kind of alkaloidal determination of recovery rates, totally 6 groups.Each group sample adds with a kind of reference substance solution an amount of respectively, and the preparation and the HPLC that carry out need testing solution by method under the need testing solution preparation item analyze.Calculate its response rate according to the amount of recording and addition.The average average recovery (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 by weighing the about 2g of each sample; A need testing solution preparation below method preparation pressed in 3 parts of the parallel titles of each sample, and carry out the analysis of 3 kinds of monoester alkaloids by above-mentioned chromatographic condition; With the same day accompanying need testing solution calculate, the result sees table 6.Reference substance, and no gallbladder Radix Aconiti Lateralis Preparata HPLC spectrogram see accompanying drawing 5, Fig. 6.
The no gallbladder Radix Aconiti Lateralis Preparata assay of table 6 self-control
According to " regulation that Chinese pharmacopoeia version in 2010 is an one, 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) the total amount meter, must not be less than 0.010%; Contain diester-type alkaloids with mesaconitine (C
33H
43NO
10), hypaconitine (C
32H
45NO
10) and aconitine (C
33H
43NO
11) the total amount meter, must not cross 0.020%.
Thus it is clear that, the no gallbladder Radix Aconiti Lateralis Preparata of all batches and do not have gallbladder Radix Aconiti Lateralis Preparata alkaloid and all meet " regulation of Chinese pharmacopoeia version in 2010.
In sum; Adopt the no gallbladder Radix Aconiti Lateralis Preparata or the Radix Aconiti Lateralis Preparata of concocting method preparation provided by the invention; Owing in concocting process, do not add edible gallbladder crust; Greatly reduce the wherein concentration of calcium ion, magnesium ion, chloride ion and other metal ions, reduced toxic and side effects, will not have gallbladder Radix Aconiti Lateralis Preparata, Radix Aconiti Lateralis Preparata simultaneously respectively by " quality standard detects under Chinese pharmacopoeia version Radix Aconiti Lateralis Preparata in 2010 item; Each item index all can reach the pharmacopeia requirement, shows that the no gallbladder Radix Aconiti Lateralis Preparata, the Radix Aconiti Lateralis Preparata that do not add edible gallbladder crust in the concocting process can reach and Radix Aconiti Lateralis Preparata, effect that Radix Aconiti Lateralis Preparata is identical.And operation in addition, and the present invention also monitors and controls no gallbladder Radix Aconiti Lateralis Preparata or Radix Aconiti Lateralis Preparata toxic composition diester-type alkaloids, heavy metal and persticide residue, for the quality and safety property of controlling no gallbladder Radix Aconiti Lateralis Preparata or Radix Aconiti Lateralis Preparata provides assurance comprehensively.
Claims (10)
1. concocting method of not having gallbladder Radix Aconiti Lateralis Preparata or Radix Aconiti Lateralis Preparata, it is characterized in that: it may further comprise the steps:
A, get fresh mud Radix Aconiti Lateralis Preparata, clean; Moderate heat keeps boiling to boil 10-20min;
B, section are soaked and are floated 20-30min, and 105 ℃ of-110 ℃ of temperature, normal pressure steams 2-10h;
C, drying promptly get.
2. concocting method according to claim 1 is characterized in that: the described steaming time of b step is 8h.
3. concocting method according to claim 1 is characterized in that: the described drying means of c step is 40 ℃-70 ℃ oven dry 17h-73h.
4. concocting method according to claim 3 is characterized in that: the described drying means of c step is 55 ℃ of oven dry 24h.
5. concocting method according to claim 1 is characterized in that: peel off crust after a step is boiled in the concocting method of described no gallbladder Radix Aconiti Lateralis Preparata, cut vertical sheet, thickness is 0.3cm-0.5cm.
6. concocting method according to claim 1 is characterized in that: not peeling after a step is boiled in the concocting method of described no gallbladder Radix Aconiti Lateralis Preparata, cut vertical sheet, thickness is 0.3cm-0.5cm.
7. the no gallbladder Radix Aconiti Lateralis Preparata or the Radix Aconiti Lateralis Preparata of any described concocting method preparation of claim 1-6.
8. no gallbladder Radix Aconiti Lateralis Preparata according to claim 7 or Radix Aconiti Lateralis Preparata is characterized in that: it contains monoester alkaloid with Benzoylmesaconine (C
31H
43NO
10), benzoyl aconine (C
32H
45NO
10) and benzoyl hypo-aconine (C
31H
43NO
9) the total amount meter, must not be less than 0.010%; Contain diester-type alkaloids with mesaconitine (C
33H
43NO
10), hypaconitine (C
32H
45NO
10) and aconitine (C
33H
43NO
11) the total amount meter, must not cross 0.020%.
9. no gallbladder Radix Aconiti Lateralis Preparata according to claim 8 or Radix Aconiti Lateralis Preparata, it is characterized in that: it contains calcium ion and is 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.
10. no gallbladder Radix Aconiti Lateralis Preparata according to claim 9 or Radix Aconiti Lateralis Preparata, it is characterized in that: 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.
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