Xiyangshen

Xiyangshen PANACIS QUINQUEFOLII RADIX

This product is the dried root of Panax quinquefolium L.They are all cultivated products.They are collected and dug in autumn,washed,dried in the sun or dried at low temperature.
[properties]the product is spindle shaped,cylindrical or conical,with a length of 3~12cm and a diameter of 0.8~2cm.The surface is light yellowish brown or yellowish white,with transverse ring lines and linear lenticular protrusions,fine and shallow longitudinal wrinkles and fibrous root marks.There are one to several lateral roots in the middle and lower part of the main root,most of which have been broken.Some have rhizomes(reed heads)at the upper end,obvious links,round or semi-circular stem marks(reed bowls),with adventitious roots(crows)or broken.Weight,solid,not easy to break,flat section,light yellow and white,slightly powdery,yellowish brown dotted resin channels can be seen on the skin,forming a ring of brownish yellow,and the wood is slightly radial.The Qi is slight and special,and the taste is slightly bitter and sweet.
[identification]take 1g of this product powder,add 25ml of methanol,heat and reflux for 30 minutes,filter,evaporate the filtrate,add 20ml of water to dissolve the residue,shake and extract the saturated n-butanol twice,25ml each time,combine the n-butanol extract,wash with water twice,10ml each time,separate the n-butanol solution,evaporate it,and add 4ml of methanol to dissolve the residue as the test solution.Another 1g of American ginseng reference material was taken and prepared into the reference material solution by the same method.Then take ginsenoside F11 control sample,ginsenoside Rb1 control sample,ginsenoside Re control sample and ginsenoside Rg1 control sample,and add methanol to prepare a solution containing 2mg per 1ml as the control solution.According to the test of thin layer chromatography(general rule 0502),absorb 2 of the above six solutionsμl.Point on the same silica gel G thin-layer plate respectively,use the lower layer solution of chloroform ethyl acetate methanol water(15:40:22:10)for 12 hours at 5~10°C as the developing agent,develop,take out,dry,spray 10%sulfuric acid ethanol solution,heat at 105°C until the spots are clear,and examine them separately under sunlight and ultraviolet light(365nm).In the chromatogram of the test sample,spots or fluorescent spots of the same color are displayed respectively at the positions corresponding to the chromatogram of the control medicinal material and the chromatogram of the control sample.
[inspection]the moisture content shall not exceed 13.0%(the second method of general rule 0832).
The total ash content shall not exceed 5.0%(general rule 2302).
Ginseng take 1g of ginseng reference material and prepare the reference material solution according to the preparation method of reference material solution under[identification].According to the test of thin layer chromatography(general rule 0502),absorb 2 samples of the test solution under[identification]and 2 samples of the above reference drug solutionμl.Point on the same silica gel G thin layer plate respectively,use the lower layer solution of chloroform methanol water(13:7:2)for 12 hours at 5~10°C as the developing agent,develop,take out,dry,spray with 10%sulfuric acid ethanol solution,heat at 105°C until the spots are clear,and inspect them under sunlight and ultraviolet light(365nm).The chromatogram of the test sample shall not show spots completely consistent with the control drug.
Heavy metals and harmful elements shall be determined according to the determination method of lead,cadmium,arsenic,mercury and copper(general rule 2321 atomic absorption spectrophotometry or inductively coupled plasma mass spectrometry).Lead shall not exceed 5mg/kg;Cadmium shall not exceed 1mg/kg;Arsenic shall not exceed 2mg/kg;Mercury shall not exceed 0.2mg/kg;Copper shall not exceed 20mg/kg.
Other organochlorine pesticide residues shall be determined by gas chromatography(general rule 0521).
Chromatographic conditions and system applicability test analysis column:capillary column(30M)with bonded cross-linked 14%cyanopropyl phenyl dimethylsiloxane as stationary liquid(dm1701 or the same type)×0.32mm×zero point two fiveμm),validation column:capillary column(30M)with bonded cross-linked 5%phenylmethylsiloxane as stationary liquid(db5 or the same type)×0.32mm×zero point two fiveμm）；63Ni ECD electron capture detector;The temperature of the injection port is 230°C,and the temperature of the detector is 300°C.There is no split injection.The column temperature is programmed temperature rise:the initial temperature is 60°C,keep it for 0.3 minutes,rise to 170°C at 60°C per minute,rise to 220°C at 10°C per minute,keep it for 10 minutes,rise to 240°C at 1°C per minute,rise to 280°C at 15°C per minute,and keep it for 5 minutes.Number of theoretical plates byα-BHC peak calculation[1]shall not be less than 1×105.The resolution of two adjacent chromatographic peaks shall be greater than 1.5.
Preparation of stock solution of mixed reference substance:accurately weigh an appropriate amount of pentachloronitrobenzene,hexachlorobenzene,heptachlor(heptachlor,epoxy heptachlor)and chlordane(CIS chlordane,trans chlordane and oxychlordane)pesticide reference substances respectively,and dissolve them with n-hexane to make them contain about 100%per 1mlμG solution.Accurately measure 1ml of each of the above reference solution,put it into the same 100ml measuring bottle,add n-hexane to the scale,and shake well;Or precisely measure 1ml of organochlorine pesticide mixed reference solution,put it into a 10ml measuring bottle,add n-hexane to the scale,and shake well to obtain(each 1ml contains 1 of each pesticide reference)μg）。
Preparation of mixed reference solution:accurately measure the stock solution of the above mixed reference,and prepare a solution containing 1ng,2ng,5ng,10NG,20ng,50NG and 100ng per 1ml with n-hexane.
Preparation of test solution:take about 5g of this product,crush it into fine powder(pass No.2 sieve),accurately weigh it,place it in a conical flask with a stopper,add 30ml of water,shake it for 10 minutes,accurately add 50ml of acetone,weigh it,ultrasonic treatment(power 300W,frequency 40KHz)for 30 minutes,cool it,weigh it again,make up the lost weight with acetone,add about 8g of sodium chloride,accurately add 25ml of dichloromethane,weigh it,Ultrasonic treatment(power 300W,frequency 40KHz)for 15 minutes,weigh again,make up the lost weight with dichloromethane,shake to fully dissolve sodium chloride,stand still,transfer to a centrifugal tube,centrifuge(3000 revolutions per minute)for 3 minutes to completely separate,transfer the organic phase to a corked conical bottle containing an appropriate amount of anhydrous sodium sulfate and place it for 30 minutes.Add 5ml of hexane into the dilute solution,shake it to the scale for about 10 minutes,dilute it to 1ml of hexane(about 1ml)with a precision shaking tube,dilute it to the normal solution,shake it for about 10 minutes,then transfer it to 1ml of dilute solution,then add it to the dilute solution for about 10 minutes.
The determination method is to precisely suck 1 sample solution and 1 mixed control solution with corresponding concentration respectivelyμl.Inject into the gas chromatograph,inject samples continuously for 3 times,take the average value of 3 times,and calculate according to the external standard method.
The content of pentachloronitrobenzene in this product shall not exceed 0.1mg/kg;Hexachlorobenzene shall not exceed 0.1mg/kg;Heptachlor(sum of heptachlor and epoxy heptachlor)shall not exceed 0.05mg/kg;Chlordane(the sum of CIS chlordane,trans chlordane and oxychlordane)shall not exceed 0.1mg/kg.
[extract]according to the hot leaching method(general rule 2201)under the alcohol soluble extract determination method,70%ethanol shall be used as the solvent,which shall not be less than 30.0%.
[content determination]determine according to high performance liquid chromatography(general rule 0512).
The chromatographic conditions and system suitability test take octadecyl silane bonded silica gel as filler;With acetonitrile as mobile phase A and 0.1%phosphoric acid solution as mobile phase B,gradient elution is carried out as specified in the following table;The detection wavelength is 203nm;The column temperature is 40℃.The number of theoretical plates shall not be less than 5000 according to ginsenoside Rb1 peak.
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Time(min)mobile phase a(%)mobile phase B(%)
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0～25 19→20 81→80
25～60 20→40 80→60
60～90 40→55 60→45
90～100 55→60 45→40
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Preparation of reference solution:take appropriate amount of Ginsenoside Rg1 reference,ginsenoside Re reference and ginsenoside Rb1 reference,weigh accurately,and add methanol to prepare a solution containing ginsenoside rg10.1mg,ginsenoside re0.4mg and ginsenoside rb11mg per 1ml.
Preparation of the test solution:take about 1g of the powder(passing No.3 sieve),weigh it precisely,place it in a conical flask with a stopper,accurately add 50ml of water saturated n-butanol,weigh it,heat it in a water bath,reflux it for extraction for 1.5 hours,cool it,weigh it again,use water saturated n-butanol to make up the lost weight,shake it well and filter it.Accurately measure 25ml of continuous filtrate,put it in an evaporating dish,evaporate it to dryness,add an appropriate amount of 50%methanol to dissolve the residue,transfer it to a 10ml measuring bottle,add 50%methanol to the scale,shake it well,filter it,and take the continuous filtrate.
The determination method accurately absorbs 10%of the control solution and 10%of the test solution respectivelyμl.Inject it into the liquid chromatograph for determination.
The total amount of Ginsenoside Rg1(c42h72o14),ginsenoside Re(c48h82o18)and ginsenoside Rb1(c54h92o23)contained in this product shall not be less than 2.0%.
Decoction pieces
[processing]remove the reed,moisten thoroughly,cut into thin slices,dry or mash when used.
[properties]the product is in oblong or quasi round flakes.The outer skin is light yellowish brown.The section is yellowish white to yellowish white,the cambium ring is brownish yellow,the skin has yellowish brown dotted resin channels,there are many and obvious near the cambium ring,and the wood is slightly radial texture.The Qi is slight and special,and the taste is slightly bitter and sweet.
[extract]the same as medicinal materials,not less than 25.0%.
[identification][inspection][content determination]are the same as those of medicinal materials.
[nature,taste and meridian returning]sweet,slightly bitter and cool.Return to heart,lung and kidney meridians.
[functions and indications]tonifying qi and nourishing Yin,clearing heat and generating fluid.It is used for Qi deficiency and yin deficiency,deficiency heat and fatigue,cough,asthma,phlegm and blood,internal heat and thirst,dry mouth and dry throat.
[dosage]6G,mixed with Decoction,another 3.
[note]it should not be used with Veratrum.
[storage]store in a cool and dry place,sealed and mothproof.