CN1709439A - Ginseng and astragalis blood glucose loucring dorpping pill, and its preparing and detecting method - Google Patents

Abstract

The present invention discloses a Shenqi sugar-reducing dripping pill preparation for effectively curing diabetes with obvious therapeutic effect. Said dripping pill preparation is made up by using 11 Chinese medicinal materials of ginseng (stem and leaf) saponin, astragalus root, rehmannia root, ophiopogon tuber, trichosanthes root, lyceum berry and others through a certain preparation process.

Description

A kind of ginseng and astragalis blood glucose loucring dorpping pill and preparation detection method thereof

Technical field

The present invention relates to a kind of Chinese medicine dripping pills for the treatment of diabetes, specifically a kind of ginseng and astragalis blood glucose loucring dorpping pill relates to the preparation method of this medicine simultaneously.

Background technology

Diabetes are a kind of complex diseases because of syndrome, be since in the body hormone of insulin deficit or antagonism insulin increase, or insulin can not be brought into normal play physiological action and a kind of syndrome of the glucose, protein and the lipid metabolic disorder that cause in target cell.It is characterized by the unusual rising of concentration of glucose and glucose in urine in the blood circulation, occur typical " three-many-one-little " symptom when blood glucose is too high, promptly repeatedly, polyuria, polyphagia and lose weight, and with fatigue and weak.Ketoacidosis, hypertonicity diabetic coma can take place in severe patient, and easily merge multiple infection.Along with the prolongation of the course of disease, its metabolism disorder can cause the chronic pathological changes of histoorgans such as eye, kidney, nerve, blood vessel and heart.If can not get timely, appropriate treatment, heart change, cerebrovascular disease, renal failure then take place, lose the sight of both eyes, situation such as lower limbs necrosis, become disable, lethal main cause.And onset diabetes rate height, the national sampling survey of 1995-1996, natural crowd's prevalence is up to 3.21% more than 20 years old, the whole nation 300,000 census of the population results in 1980, prevalence 4.21% more than 60 years old, single Jiangsu elderly population diabetes, impaired glucose tolerance prevalence then are respectively 14.49% and 10.21%, and no matter are developed country or developing country, and the sickness rate of diabetes is all rising year by year.

Mostly the medicine of clinical treatment 2 types is chemicals, widely used sulphanylureas, biguanides, other antidiabetic drugs and the adjuvant drug of being broadly divided into except that insulin at present.The sulfonylureas drugs for diabetes thing is topmost Remedies for diabetes.Can make that hepatic glycogen is synthetic to be increased,, surrounding tissue be strengthened to the sensitivity of insulin, the picked-up of glucose is increased, thereby reach the effect of blood sugar lowering again by the effect behind pair cell receptor or the receptor.But more easily cause untoward reaction such as hypoglycemia, granulocytopenia and cardiovascular disease.Biguanides antidiabetic drug heavy dose can cause digestive tract reaction, has the patient of pathological changes easily to cause lactic acidosis at lung, liver, kidney.Bring hidden danger for the extensive patients drug safety, for a change this situation for a long time, attempts treating with protocol in the plant clinically always.The traditional Chinese medical science is consistent to the cause of disease view of diabetes, thinks it mainly is that surfeit delicious food, overaction of the five emotions, chamber do not save, the dry and not enough Several Factors of natural endowment of calentura fire.

The treatment that current SHENQI JIANGTANG preparation clinically is widely used in type ii diabetes obtains curative effect preferably, and has no side effect, and promotional value is widely arranged; The SHENQI JIANGTANG oral formulations of present clinical use is still based on oral liquid, granule, capsule, tablet, because dosage form itself, it exists following problem:

It is few that oral liquid has dosage, easily takes, absorb fast, advantages such as good effect.But in real work, we find that the SHENQI JIANGTANG oral liquid is prone to muddiness, flocculent deposit equistability problem in storage process.Astragaloside, ginsenoside belong to saponins simultaneously, facile hydrolysis, and active ingredient is damaged, downgrade.And carry, take inconvenience, production cost height.

Tablet, capsule exist that bioavailability is low, onset waits problem slowly.

The first pass effect problem.First pass effect (First Pass Effect) claim the first pass effect again.Oral drugs after gastrointestinal absorption, at first through portal vein to liver, some medicine metabolic inactivation very easily the time by mucosa and liver, major part is destroyed for the first time by liver the time, enters sanguimotor effective dose and reduces, drug effect reduces.Oral liquid, capsule, tablet and granule produce first pass effect owing to the reason of dosage form itself nearly all absorbs in gastrointestinal tract, make to enter sanguimotor effective dose minimizing, and drug effect reduces.

At the problem of above existence, for make the SHENQI JIANGTANG preparation clinically better, clearer and more definite application, we need a kind of determined curative effect, the little SHENQI JIANGTANG preparation easy to carry of consumption to satisfy the clinical application needs.

Summary of the invention

The objective of the invention is to overcome above the deficiencies in the prior art, a kind of efficient, quick-acting SHENQI JIANGTANG preparation is provided, another object of the present invention provides the preparation detection method of this Chinese medicine preparation.

For achieving the above object, we have adopted following technical scheme:

Chinese medicine dripping pills of the present invention is to be made by the raw material of following weight ratio:

Ginsenoside 4-8 weight portion Radix Astragali 80-150 weight portion Radix Rehmanniae 150-250 weight portion

Radix Ophiopogonis 45-80 weight portion Radix Trichosanthis 40-80 weight portion Fructus Lycii 80-160 weight portion

Fructus Schisandrae Chinensis 40-80 weight portion Rhizoma Dioscoreae 40-80 weight portion Fructus Rubi 20-50 weight portion

Poria 40-80 weight portion Rhizoma Alismatis 40-80 weight portion.

The weight ratio of the raw material of Chinese medicine composition of the present invention is preferably:

Ginsenoside's 6 weight portion Radixs Astragali 124 weight portion Radix Rehmanniae 186 weight portions

Radix Ophiopogonis 62 weight portion Radix Trichosanthis, 62 weight portion Fructus Lyciis, 124 weight portions

Fructus Schisandrae Chinensis 62 weight portion Rhizoma Dioscoreaes 62 weight portion Fructus Rubies 31 weight portions

Poria 62 weight portion Rhizoma Alismatis 62 weight portions.

In order to make this product make our required drop pill, in the preparation process, need to add various required adjuvants, in the adjuvant we mainly select Polyethylene Glycol wherein extract and adjuvant Polyethylene Glycol weight ratio be 1: 1-1: 10; Both are preferably ratio: 1: 2-1: 5; Wherein Polyethylene Glycol be polyethylene glycol 6000 or with the two mixture of Macrogol 4000, be preferably Macrogol 4000 and polyethylene glycol 6000 1: 1-1: 5 mixture; Except that Polyethylene Glycol, also can add adjuvants such as tween, soft phospholipid, glycerin gelatine.Every drop pill is heavy: 30-100mg.

Mainly containing effective component content in the drop pill of the present invention is:

Contain in every gram drop pill: ginsenoside Re 0.2-20mg,

Contain in every gram drop pill: astragaloside 0.04-5mg.

The assay method of above-mentioned effective ingredient in drop pill of the present invention is:

(1) ginsenoside Re's assay method is:

The preparation of reference substance solution: it is an amount of that precision takes by weighing ginsenoside Re's reference substance, adds methanol and make the solution that contains ginsenoside Re 0.2-0.8mg among every 1ml respectively, in contrast product solution;

The preparation of need testing solution: get this product 1-10 gram, the accurate title, decide, and adds methanol 10-50ml, dissolving, filter, volatilize, be dissolved in water, add water saturated n-butyl alcohol 25-100ml extraction 2-6 time, merge n-butanol extracting liquid, add the ammonia solution triplication, shake up, place, divide and get upper solution, evaporate to dryness, residue add methanol makes dissolving, quantitatively moves in the 2-10ml measuring bottle, add methanol and be diluted to scale, shake up, promptly;

Chromatographic condition: with octadecylsilane chemically bonded silica is filler; Volume ratio is that 99: 400 acetonitrile-0.05% phosphoric acid solution is a mobile phase; Detect wavelength 203nm;

Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject hplc determination;

(2) assay method of astragaloside is:

Chromatographic condition: octadecylsilane chemically bonded silica is a filler; Evaporative light scattering detector;

Mobile phase: ratio is acetonitrile-water-oxolane of 33: 67: 4;

The preparation of reference substance solution: get the astragaloside reference substance and add methanol and make the solution that every 1ml contains 0.1-2mg, shake up;

The preparation of need testing solution: get the about 1-5 gram of this product, the accurate title, decide, and adds water 10-50ml dissolving, filter, filtrate is used defat with petroleum ether 1-3 time, and water liquid extracts (each 10-50ml) 2-6 time with water saturated n-butyl alcohol jolting, merge n-butanol extracting liquid, extract 1-2 time, each 5-40ml with ammonia solution, discard ammonia solution, the water 10-40ml saturated with n-butyl alcohol washes, and discards water liquid, n-butyl alcohol liquid evaporate to dryness, residue adds water 5-10ml makes dissolving, puts coldly, passes through D ₁₀₁Type macroporous adsorptive resins (internal diameter 1.5cm, long 18cm) is with water elution, discard water liquid, reuse 10-40% ethanol 10-100ml eluting discards ethanol elution, continue with 50-90% ethanol 50-150ml eluting, collect eluent, evaporate to dryness is with dissolve with methanol and be transferred in the 2-10ml measuring bottle, add methanol to scale, shake up, filter, promptly.

The preparation method of drop pill of the present invention is prepared by following steps:

A uses warm water lixiviate 1-3 time Radix Ophiopogonis, and each 0.5-3 hour, merge lixiviating solution, filter, filtrate is concentrated into the thick paste that relative density is 1.03-1.40;

B Fructus Schisandrae Chinensis 40-70% ethanol, percolation, percolate reclaim ethanol, are concentrated into thick paste;

C Fructus Lycii, the Radix Astragali, Radix Rehmanniae, Rhizoma Alismatis, Rhizoma Dioscoreae, Radix Trichosanthis, Fructus Rubi, Poria water decoct 1-4 time, each 0.5-3 hour, merging decoction liquor, filtration, filtrate, to be concentrated into relative density be 1.20 thick paste, adding ethanol makes and contains the alcohol amount and be 40%-80%, leave standstill, the leaching supernatant, reclaim ethanol, concentrate

D merges drying, pulverizing and ginsenoside with above-mentioned extractum and merges, mixing, add the extract powder mixing after getting adjuvant Polyethylene Glycol heating and melting, move in the drop pill machine storage tank, in the water dropper temperature is under the 70-90 ℃ of condition, with 60-150 drip/minute the speed of dripping splash in liquid paraffin or the dimethicone, remove liquid coolant, select ball, promptly.

Drug treatment of diabetic of the present invention has better curative effect.For showing medicine of the present invention to the treatment of diabetes effect, we have done a large amount of experimentatioies, below experimental example be used to further specify the present invention.

Clinical research

(1) case is selected: Chinese and western medicine diagnostic criteria, criterion of therapeutical effect are all undertaken by " technological guidance's principle of new drug (Chinese medicine) treatment diabetes (diabetes) clinical research ".

1, Western medicine diagnose standard (WHO expert consulting report in 1999)

(1) diabetes fasting glucose (FPG) 〉=7.0mmol/L (126ml/dl); Or back 2 hours blood glucose (2HPG) 〉=11.1mmol/L (200mg/dl) of clothes sugar in the carbohydrate tolerance test (OGTT); Or random blood sugar 〉=11.1mmol/L (200mg/dl).

(2) carbohydrate tolerance injury (IGT) fasting glucose (FPG)＜7.0mmol/L (126ml/dl), and back 2 hours blood glucose 〉=7.8mmol/L (140mg/dl) of clothes sugar in the carbohydrate tolerance test.

(3) fasting glucose injury (IGG) 6.1mmol/L (110mg/dl)≤fasting glucose＜7.0mmol/L (126mg/dl), back 2 hours blood glucose＜7.8mmol/L (140mg/dl) of clothes sugar in the carbohydrate tolerance test.

2, Syndrome in TCM marquis diagnostic criteria

(1) intense heat due to deficiency of YIN card

Main symptom: dry mouth and throat, vexed fear heat.

Inferior card: thirst and desire for cold drink, polyorexia, the red constipation of urinating.

Tongue arteries and veins: red tongue with yellow fur, thready and rapid pulse, or thin stringy and rapid pulse.

(2) syndrome of deficiency of both qi and yin

Main symptom: dry mouth and throat, fatigue and weakness.

Inferior card: polyorexia, thirst and liking drink, the lazy speech of breathing hard, dysphoria with feverish sensation in the chest palms and soles, palpitation and insomnia, the red constipation of urinating.

Tongue arteries and veins: red tongue with a little fluid liquid, thin fur or flower stripping, thready and rapid pulse without strength, or thin stringy and rapid pulse.

(3) deficiency syndrome of both YIN and YANG

Main symptom: spiritlessness and weakness, dry mouth and throat, the acid of waist knee joint is cold, or brothers fear cold, nocturia.

Inferior card: dizziness and blurred vision, palpitation and insomnia, the spontaneous perspiration susceptible, the lazy speech of breathing hard, face limbs edema, the turbid foam of frequent micturition, or the urine amount is few, impotence in male, and woman's libido is cold and detached, and it is rare dried uncomfortable to defecate.

The tongue arteries and veins: corpulent tongue is big, red trace is arranged, thready and rapid pulse without strength.

(2) testing program

The case grouping: the pairing grouping, 373 examples are organized in treatment, wherein select typical intense heat due to deficiency of YIN to demonstrate,prove 38 examples, deficiency of both QI and YIN 100 examples;

Deficiency of both YIN and YANG 31 examples, matched group 108 examples.

Test drug:

Preparation of the present invention (ginseng and astragalis blood glucose loucring dorpping pill), Shandong southern Shandong pharmaceutical factory laboratory provides.Obey the granule 2/3 that the crude drug amount is at every turn.

SHENQI JIANGTANG KELI: southern Shandong pharmaceutical factory in Shandong provides,

Method: promptly award the ginseng and astragalis blood glucose loucring dorpping pill treatment after the patient of treatment group is in hospital, every day 3 times, each to obey the crude drug amount be 2/3 of granule.The patient of matched group promptly gives SHENQI JIANGTANG KELI after being in hospital, and 2 months is a course of treatment, and complicated hypertension adds with enalapril, nitrendipine, merges coronary heart disease and adds Radix Salviae Miltiorrhizae drop pill, sorbitrate.Look into fasting glucose (GLU), triglyceride (TG), cholesterol (TC), glucose in urine etc. before and after the medication respectively.

Efficacy determination:

(1) disease curative effect determinate standard

(1) clinical recovery: tcm clinical practice symptom, sign disappear or basic the disappearance, and the syndrome integration reduces 〉=90%.(2) produce effects: tcm clinical practice symptom, sign are obviously improved, and the syndrome integration reduces 〉=70%.

(3) effective: tcm clinical practice symptom, sign all take a favorable turn, and the syndrome integration reduces 〉=30%.

(4) invalid: tcm clinical practice symptom, sign all do not have obvious improvement, even increase the weight of, the syndrome integration reduces less than 30%.

Annotate: computing formula (nimodipine method) is: [integration before (integration before the treatment-treatment back integration) ÷ treatment] * 100%.

(2) mainly detect index (blood glucose) curative effect determinate standard

(1) produce effects: fasting glucose and 2 hours after the meal blood glucose drop to normal range; Or fasting glucose and 2 hours after the meal blood glucose values descend and surpass 40% before the treatment, and the glycolated hemoglobin value drops to normally, or descend surpass treatment preceding 30%.

(2) effective: fasting glucose and 2 hours after the meal blood glucose drop-out values surpass 20% before the treatment, but do not reach the produce effects standard, and the glycolated hemoglobin drop-out value surpasses 10% before the treatment, but does not reach the produce effects standard.

(3) invalid: tcm clinical practice symptom, sign all do not have obvious improvement, even increase the weight of, the syndrome integration reduces less than 30%, fasting glucose and 2 hours after the meal blood glucose do not have decline, or descend and not reach effective standard, glycolated hemoglobin value does not down have and descends, or does not reach effective standard.

(3) curative effect of disease criterion

(1) produce effects: tcm clinical practice symptom, sign are obviously improved, and the syndrome integration reduces 〉=70%; Fasting glucose and 2 hours after the meal blood glucose drop to normal range; Or fasting glucose and 2 hours after the meal blood glucose values descend and surpass 40% before the treatment, and the glycolated hemoglobin value drops to below 6.2%, or descend and surpass 30% before the treatment.

(3) effective: tcm clinical practice symptom, sign all take a favorable turn, the syndrome integration reduces 〉=30%, and fasting glucose reaches 2 hours after the meal blood glucose drop-out values above 20% before treating, but does not reach the produce effects standard, the glycolated hemoglobin drop-out value surpasses 10% before the treatment, but does not reach the produce effects standard.。

(4) invalid: fasting glucose and 2 hours after the meal blood glucose do not have decline, or descend and do not reach effective standard, and glycolated hemoglobin value does not down have and descends, or does not reach effective standard.

The result:

1, disease curative effect: finish the back course of treatment and observe treatment group result: intense heat due to deficiency of YIN is demonstrate,proved wherein produce effects 12 examples (31.6%) of 38 examples, effective 16 examples (42.1%), invalid 10 examples (26.3%), total effective rate 73.7%; Deficiency of both QI and YIN 100 examples are produce effects 44 examples (44%) wherein, effective 48 examples (48%), invalid 8 examples (8%), total effective rate 92%; Deficiency of both YIN and YANG 31 examples are produce effects 10 examples (32.3%) wherein, effective 13 examples (41.9%), invalid 8 examples (25.8%), total effective rate 74.2%.Matched group: intense heat due to deficiency of YIN is demonstrate,proved wherein produce effects 3 examples (25%) of 12 examples, effective 5 examples (41.7%), invalid 4 examples (33.3%), total effective rate 66.7%; Deficiency of both QI and YIN 33 examples are produce effects 13 examples (39.4%) wherein, effective 14 examples (42.4%), invalid 5 examples (15.2%), total effective rate 84.8%; Deficiency of both YIN and YANG 8 examples are produce effects 3 examples (37.5%) wherein, effective 4 examples (50%), invalid 1 example (12.5%), total effective rate 87.5%.As a result, see Table 1.

Table 1 ginseng is luxuriant falls drop pill and the sugared granule curative effect to type ii diabetes Chinese medical discrimination typing

Disease curative effect example digital display is imitated the total significant figure (rate) of number (rate) significant figure (rate) invalid number (rate)

Control intense heat due to deficiency of YIN 38 12 (31.6%) 16 (42.1%) 10 (26.3%) 28 (73.7%)

Treat deficiency of both QI and YIN 100 44 (44%) 48 (48%) 8 (8%) 92 (92%)

Group deficiency of both YIN and YANG 31 10 (32.3%) 13 (41.9%) 8 (25.8%) 12 (74.2%)

Total example several 169 62 81 26 132

To intense heat due to deficiency of YIN 12 3 (39.4%) 5 (41.7%) 4 (33.3%) 8 (66.7%)

According to deficiency of both QI and YIN 33 13 (39.4%) 14 (42.4%) 5 (15.2%) 27 (84.8%)

Group deficiency of both YIN and YANG 83 (37.5%) 4 (50%) 1 (12.5%) 7 (87.5%)

Total example several 53 19 23 10 42

2, mainly detect the index curative effect:

By treatment group and matched group are mainly detected index glucose in urine, cholesterol and triglyceride efficacy determination result such as table 2

The influence of table 2 ginseng and astragalis blood glucose loucring dorpping pill and control Group II diabetes mellitus type glucose in urine and blood fat

Glucose in urine cholesterol triglyceride

Treatment group % treatment of control group group treatment of control group group matched group

Produce effects (%) 35.12 33.33 23.06 23.81 28.69 28.70

Effective (%) 37.27 35.78 13.94 13.89 20.11 20.37

Invalid (%) 23.59 23.1 48.26 49.07 31.90 31.48

Increase the weight of (%) 4.04 7.79 14.74 13.23 19.30 19.45

Ginseng and astragalis blood glucose loucring dorpping pill and control Group II diabetes mellitus type blood glucose influence result such as table 3

The influence of table 3 ginseng and astragalis blood glucose loucring dorpping pill and control Group II diabetes mellitus type blood glucose

Blood glucose drop-out value treatment group matched group

3 months routine number % of 2 months routine number % 2 months routine number % of 3 months routine number %

＞40％ 253 67.83 69 70.41 69 63.89 52 59.77

20％ 86 23.06 10 10.2 13 12.04 7 8.05

10％ 12 3.22 6 6.12 8 7.41 10 11.49

0 3 0.80 7 7.14 11 10.19 6 6.90

＜-10 12 3.22 4 4.08 3 2.78 5 5.75

-20 7 1.88 2 2.04 5 4.63 6 6.90

The total rate of descent 94.11 86.73 83.34 79.31 of blood glucose

Total example several 373 98 108 87

Learn from last table: no matter be to use ginseng and astragalis blood glucose loucring dorpping pill; also be to use SHENQI JIANGTANG KELI all to have to regulate acceptor levels effect (in help carbohydrate metabolism normalization direction), lipid peroxide and the cell receptor behind stress hyperglycemia, the damaging hyperglycemia of islets of langerhans, the abnormal carbohydrate metabolism had the adjusting metabolism.And can the growth and the metabolism of human embryonic lung diploid fibroblast be exerted an influence, particularly to for the propagation of cell and endocellular sugar unit content the normotopia facilitation being arranged evening.

Ginseng and astragalis blood glucose loucring dorpping pill is to develop on the basis of SHENQI JIANGTANG KELI, but less relatively (the reducing 1/3rd) of the active component of its medicine; But the curative effect of medicine does not weaken, and strengthens to some extent on the contrary, can think that therefore preparation of the present invention can play the effect identical with former dosage form under the situation of taking the minimizing of crude drug amount, produced beyond thought effect.

Following embodiment is further openly the present invention, need to prove that these embodiment only for optimal way of the present invention, do not limit the scope of protection of present invention.

Embodiment 1

Ginsenoside 6g Radix Astragali 124g Radix Rehmanniae 186g

Radix Ophiopogonis 62g Radix Trichosanthis 62g Fructus Lycii 124g

Fructus Schisandrae Chinensis 62g Rhizoma Dioscoreae 62g Fructus Rubi 31g

Poria 62g Rhizoma Alismatis 62g.

Method for making: a Radix Ophiopogonis is with warm water lixiviate 2 times, and each 2 hours, merge lixiviating solution, filter, it is 1.20 thick paste that filtrate is concentrated into relative density;

B Fructus Schisandrae Chinensis 50% ethanol, percolation, percolate reclaim ethanol, are concentrated into thick paste;

C Fructus Lycii, the Radix Astragali, Radix Rehmanniae, Rhizoma Alismatis, Rhizoma Dioscoreae, Radix Trichosanthis, Fructus Rubi, Poria water decoct 2 times, each 1.5 hours, merging decoction liquor, filtration, filtrate, to be concentrated into relative density be 1.20 thick paste, add ethanol and make that to contain the alcohol amount be 60%, leave standstill, the leaching supernatant, reclaim ethanol, concentrate

D merges drying, pulverizing and ginsenoside with above-mentioned extractum and merges, mixing gets extract powder 90g, add the extract powder mixing after getting adjuvant Polyethylene Glycol PEG6000 900g heating and melting, move in the drop pill machine storage tank, in the water dropper temperature is under 80 ℃ of conditions, splashes in the liquid coolant liquid paraffin with 80 droplets/minute the speed of dripping, and removes liquid coolant, select ball, promptly.

Assay method is:

(1) ginsenoside Re's assay method is:

The preparation of reference substance solution: it is an amount of that precision takes by weighing ginsenoside Re's reference substance, adds methanol and make the solution that contains ginsenoside Re 0.2mg among every 1ml, in contrast product solution;

The preparation of need testing solution: get this product 1 gram, the accurate title, decide, and adds methanol 10ml, dissolving, filter, volatilize, be dissolved in water, add water saturated n-butyl alcohol 25ml extraction 2 times, merge n-butanol extracting liquid, add the ammonia solution triplication, shake up, place, divide and get upper solution, evaporate to dryness, residue add methanol makes dissolving, quantitatively moves in the 2ml measuring bottle, add methanol and be diluted to scale, shake up, promptly;

Chromatographic condition: with octadecylsilane chemically bonded silica is filler; Volume ratio is that 99: 400 acetonitrile-0.05% phosphoric acid solution is a mobile phase; Detect wavelength 203nm;

Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject hplc determination;

(2) assay method of astragaloside is:

Chromatographic condition: octadecylsilane chemically bonded silica is a filler; Evaporative light scattering detector;

Mobile phase: ratio is acetonitrile-water-oxolane of 33: 67: 4;

The preparation of reference substance solution: get the astragaloside reference substance and add methanol and make the solution that every 1ml contains 0.1mg, shake up;

The preparation of need testing solution: get about 1 gram of this product, the accurate title, decide, and adds water 10ml dissolving, filter, filtrate is used defat with petroleum ether 1 time, and water liquid extracts (each 10ml) 2 times with water saturated n-butyl alcohol jolting, merge n-butanol extracting liquid, extract 1 time, each 5ml with ammonia solution, discard ammonia solution, the water 10ml saturated with n-butyl alcohol washes, and discards water liquid, n-butyl alcohol liquid evaporate to dryness, residue adds water 5mL makes dissolving, puts coldly, passes through D ₁₀₁Type macroporous adsorptive resins (internal diameter 1.5cm, long 18cm) is with water elution, discard water liquid, reuse 10% ethanol 10ml eluting discards ethanol elution, continue with 50% ethanol 50ml eluting, collect eluent, evaporate to dryness is with dissolve with methanol and be transferred in the 2ml measuring bottle, add methanol to scale, shake up, filter, promptly.

The result: every gram drop pill contains ginsenoside Re 0.2mg, contains astragaloside 0.04mg.

Embodiment 2

Ginsenoside 4g Radix Astragali 150g Radix Rehmanniae 250g

Radix Ophiopogonis 80g Radix Trichosanthis 80g Fructus Lycii 160g

Fructus Schisandrae Chinensis 80g Rhizoma Dioscoreae 80g Fructus Rubi 50g

Poria 80g Rhizoma Alismatis 80g

Method for making: a Radix Ophiopogonis is with warm water lixiviate 3 times, and each 3 hours, merge lixiviating solution, filter, it is 1.40 thick paste that filtrate is concentrated into relative density;

B Fructus Schisandrae Chinensis 70% ethanol, percolation, percolate reclaim ethanol, are concentrated into thick paste;

C Fructus Lycii, the Radix Astragali, Radix Rehmanniae, Rhizoma Alismatis, Rhizoma Dioscoreae, Radix Trichosanthis, Fructus Rubi, Poria water decoct 4 times, and each 3 hours, merging decoction liquor, filtration, filtrate, to be concentrated into relative density be 1.20 thick paste, add ethanol and make that to contain the alcohol amount be 80%, leave standstill, the leaching supernatant, reclaim ethanol, concentrate

D merges drying, pulverizing and ginsenoside with above-mentioned extractum and merges, mixing gets extract powder 175g, get adjuvant Macrogol 4000 87.5g, polyethylene glycol 6000 87.5g adds the extract powder mixing behind the heating and melting, move in the drop pill machine storage tank, in the water dropper temperature is under 70 ℃ of conditions, splashes in the dimethicone with 60 droplets/minute the speed of dripping, and removes liquid coolant, select ball, promptly.

Assay method is:

(1) ginsenoside Re's assay method is:

The preparation of reference substance solution: it is an amount of that precision takes by weighing ginsenoside Re's reference substance, adds methanol and make the solution that contains ginsenoside Re 0.8mg among every 1ml, in contrast product solution;

The preparation of need testing solution: get this product 10 grams, the accurate title, decide, and adds methanol 50ml, dissolving, filter, volatilize, be dissolved in water, add water saturated n-butyl alcohol 100ml extraction 6 times, merge n-butanol extracting liquid, add the ammonia solution triplication, shake up, place, divide and get upper solution, evaporate to dryness, residue add methanol makes dissolving, quantitatively moves in the 10ml measuring bottle, add methanol and be diluted to scale, shake up, promptly;

Chromatographic condition: with octadecylsilane chemically bonded silica is filler; Volume ratio is that 99: 400 acetonitrile-0.05% phosphoric acid solution is a mobile phase; Detect wavelength 203nm;

Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject hplc determination;

(2) assay method of astragaloside is:

Chromatographic condition: octadecylsilane chemically bonded silica is a filler; Evaporative light scattering detector;

Mobile phase: ratio is acetonitrile-water-oxolane of 33: 67: 4;

The preparation of reference substance solution: get the astragaloside reference substance and add methanol and make the solution that every 1ml contains 2mg, shake up;

The preparation of need testing solution: get about 5 grams of this product, the accurate title, decide, and adds water 50ml dissolving, filter, filtrate is used defat with petroleum ether 3 times, and water liquid extracts (each 50ml) 6 times with water saturated n-butyl alcohol jolting, merge n-butanol extracting liquid, extract 2 times, each 40ml with ammonia solution, discard ammonia solution, the water 40ml saturated with n-butyl alcohol washes, and discards water liquid, n-butyl alcohol liquid evaporate to dryness, residue adds water 10mL makes dissolving, puts coldly, passes through D ₁₀₁Type macroporous adsorptive resins (internal diameter 1.5cm, long 18cm) is with water elution, discard water liquid, reuse 40% ethanol 100ml eluting discards ethanol elution, continue with 90% ethanol 150ml eluting, collect eluent, evaporate to dryness is with dissolve with methanol and be transferred in the 10ml measuring bottle, add methanol to scale, shake up, filter, promptly.

The result: every gram drop pill contains ginsenoside Re 2mg, contains astragaloside 5mg.

Embodiment 3

Ginsenoside 8g Radix Astragali 80g Radix Rehmanniae 250g

Radix Ophiopogonis 80g Radix Trichosanthis 80g Fructus Lycii 160g

Fructus Schisandrae Chinensis 80g Rhizoma Dioscoreae 80g Fructus Rubi 50g

Poria 80g Rhizoma Alismatis 80g

Method for making: a Radix Ophiopogonis is with warm water lixiviate 1 time, and each 3 hours, merge lixiviating solution, filter, it is 1.30 thick paste that filtrate is concentrated into relative density;

B Fructus Schisandrae Chinensis 50% ethanol, percolation, percolate reclaim ethanol, are concentrated into thick paste;

C Fructus Lycii, the Radix Astragali, Radix Rehmanniae, Rhizoma Alismatis, Rhizoma Dioscoreae, Radix Trichosanthis, Fructus Rubi, Poria water decoct 3 times, each 1.5 hours, merging decoction liquor, filtration, filtrate, to be concentrated into relative density be 1.20 thick paste, add ethanol and make that to contain the alcohol amount be 50%, leave standstill, the leaching supernatant, reclaim ethanol, concentrate

D merges drying, pulverizing and ginsenoside with above-mentioned extractum and merges, mixing gets extract powder 210g, add the extract powder mixing after getting adjuvant Macrogol 4000 70g, polyethylene glycol 6000 350g heating and melting, move in the drop pill machine storage tank, in the water dropper temperature is under 90 ℃ of conditions, splashes in the liquid coolant dimethicone with 150 droplets/minute the speed of dripping, and removes liquid coolant, select ball, promptly.

Assay:

(1) ginsenoside Re's assay method is:

The preparation of reference substance solution: it is an amount of that precision takes by weighing ginsenoside Re's reference substance, adds methanol and make the solution that contains ginsenoside Re 0.4mg among every 1ml, in contrast product solution;

The preparation of need testing solution: get this product 5 grams, the accurate title, decide, and adds methanol 25ml, dissolving, filter, volatilize, be dissolved in water, add water saturated n-butyl alcohol 50ml extraction 4 times, merge n-butanol extracting liquid, add the ammonia solution triplication, shake up, place, divide and get upper solution, evaporate to dryness, residue add methanol makes dissolving, quantitatively moves in the 5ml measuring bottle, add methanol and be diluted to scale, shake up, promptly;

Chromatographic condition: with octadecylsilane chemically bonded silica is filler; Volume ratio is that 99: 400 acetonitrile-0.05% phosphoric acid solution is a mobile phase; Detect wavelength 203nm;

Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject hplc determination;

(2) assay method of astragaloside is:

Chromatographic condition: octadecylsilane chemically bonded silica is a filler; Evaporative light scattering detector;

Mobile phase: ratio is acetonitrile-water-oxolane of 33: 67: 4;

The preparation of reference substance solution: get the astragaloside reference substance and add methanol and make the solution that every 1ml contains 0.5mg, shake up;

The preparation of need testing solution: get about 3 grams of this product, the accurate title, decide, and adds water 25ml dissolving, filter, filtrate is used defat with petroleum ether 2 times, and water liquid extracts (each 10-50ml) 4 times with water saturated n-butyl alcohol jolting, merge n-butanol extracting liquid, extract 2 times, each 25ml with ammonia solution, discard ammonia solution, the water 40ml saturated with n-butyl alcohol washes, and discards water liquid, n-butyl alcohol liquid evaporate to dryness, residue adds water 10mL makes dissolving, puts coldly, passes through D ₁₀₁Type macroporous adsorptive resins (internal diameter 1.5cm, long 18cm) is with water elution, discard water liquid, reuse 30% ethanol 50ml eluting discards ethanol elution, continue with 70% ethanol 100ml eluting, collect eluent, evaporate to dryness is with dissolve with methanol and be transferred in the 5ml measuring bottle, add methanol to scale, shake up, filter, promptly.

The result: every gram drop pill contains ginsenoside Re 20mg, contains astragaloside 5mg.

Embodiment 4

Ginsenoside 8g Radix Astragali 150g Radix Rehmanniae 150g

Radix Ophiopogonis 80g Radix Trichosanthis 80g Fructus Lycii 160g

Fructus Schisandrae Chinensis 80g Rhizoma Dioscoreae 80g Fructus Rubi 50g

Poria 80g Rhizoma Alismatis 80g

Method for making: a Radix Ophiopogonis is with warm water lixiviate 3 times, and each 2.5 hours, merge lixiviating solution, filter, it is 1.20 thick paste that filtrate is concentrated into relative density;

B Fructus Schisandrae Chinensis 55% ethanol, percolation, percolate reclaim ethanol, are concentrated into thick paste;

C Fructus Lycii, the Radix Astragali, Radix Rehmanniae, Rhizoma Alismatis, Rhizoma Dioscoreae, Radix Trichosanthis, Fructus Rubi, Poria water decoct 2 times, and each 1 hour, merging decoction liquor, filtration, filtrate, to be concentrated into relative density be 1.20 thick paste, add ethanol and make that to contain the alcohol amount be 70%, leave standstill, the leaching supernatant, reclaim ethanol, concentrate

D merges drying, pulverizing and ginsenoside with above-mentioned extractum and merges, mixing gets extract powder 160g, get adjuvant Macrogol 4000 200g polyethylene glycol 6000 600g, adding the extract powder mixing behind the heating and melting, move in the drop pill machine storage tank, is under 85 ℃ of conditions in the water dropper temperature, the speed of dripping with 90 droplets/minute splashes in the liquid coolant liquid paraffin, remove liquid coolant, select ball, promptly.Assay:

(1) ginsenoside Re's assay method is:

The preparation of reference substance solution: it is an amount of that precision takes by weighing ginsenoside Re's reference substance, adds methanol and make the solution that contains ginsenoside Re 0.6mg among every 1ml, in contrast product solution;

The preparation of need testing solution: get this product 2 grams, the accurate title, decide, and adds methanol 20ml, dissolving, filter, volatilize, be dissolved in water, add water saturated n-butyl alcohol 50ml extraction 5 times, merge n-butanol extracting liquid, add the ammonia solution triplication, shake up, place, divide and get upper solution, evaporate to dryness, residue add methanol makes dissolving, quantitatively moves in the 5ml measuring bottle, add methanol and be diluted to scale, shake up, promptly;

Chromatographic condition: with octadecylsilane chemically bonded silica is filler; Volume ratio is that 99: 400 acetonitrile-0.05% phosphoric acid solution is a mobile phase; Detect wavelength 203nm;

Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject hplc determination;

(2) assay method of astragaloside is:

Chromatographic condition: octadecylsilane chemically bonded silica is a filler; Evaporative light scattering detector;

Mobile phase: ratio is acetonitrile-water-oxolane of 33: 67: 4;

The preparation of reference substance solution: get the astragaloside reference substance and add methanol and make the solution that every 1ml contains 1mg, shake up;

The preparation of need testing solution: get about 2 grams of this product, the accurate title, decide, and adds water 20ml dissolving, filter, filtrate is used defat with petroleum ether 3 times, and water liquid extracts (each 25ml) 6 times with water saturated n-butyl alcohol jolting, merge n-butanol extracting liquid, extract 2 times, each 20ml with ammonia solution, discard ammonia solution, the water 30ml saturated with n-butyl alcohol washes, and discards water liquid, n-butyl alcohol liquid evaporate to dryness, residue adds water 10mL makes dissolving, puts coldly, passes through D ₁₀₁Type macroporous adsorptive resins (internal diameter 1.5cm, long 18cm) is with water elution, discard water liquid, reuse 40% ethanol 80ml eluting discards ethanol elution, continue with 70% ethanol 100ml eluting, collect eluent, evaporate to dryness is with dissolve with methanol and be transferred in the 5ml measuring bottle, add methanol to scale, shake up, filter, promptly.

The result: every gram drop pill contains ginsenoside Re 20mg, contains astragaloside 0.04mg.

Embodiment 5

Ginsenoside 8g Radix Astragali 150g Radix Rehmanniae 250g

Radix Ophiopogonis 45g Radix Trichosanthis 80g Fructus Lycii 160g

Fructus Schisandrae Chinensis 80g Rhizoma Dioscoreae 80g Fructus Rubi 50g

Poria 80g Rhizoma Alismatis 80g

Method for making: a Radix Ophiopogonis is with warm water lixiviate 2 times, and each 2 hours, merge lixiviating solution, filter, it is 1.40 thick paste that filtrate is concentrated into relative density;

B Fructus Schisandrae Chinensis 50% ethanol, percolation, percolate reclaim ethanol, are concentrated into thick paste;

C Fructus Lycii, the Radix Astragali, Radix Rehmanniae, Rhizoma Alismatis, Rhizoma Dioscoreae, Radix Trichosanthis, Fructus Rubi, Poria water decoct 3 times, and each 2 hours, merging decoction liquor, filtration, filtrate, to be concentrated into relative density be 1.20 thick paste, add ethanol and make that to contain the alcohol amount be 70%, leave standstill, the leaching supernatant, reclaim ethanol, concentrate

D merges drying, pulverizing and ginsenoside with above-mentioned extractum and merges, mixing gets extract powder 100g, add the extract powder mixing after getting adjuvant polyethylene glycol 6000 800g, tween 80 100g heating and melting, move in the drop pill machine storage tank, in the water dropper temperature is under 750 ℃ of conditions, splashes in the liquid coolant dimethicone with 130 droplets/minute the speed of dripping, and removes liquid coolant, select ball, promptly.Content assaying method:

(1) ginsenoside Re's assay method is:

The preparation of reference substance solution: it is an amount of that precision takes by weighing ginsenoside Re's reference substance, adds methanol and make the solution that contains ginsenoside Re 0.4mg among every 1ml, in contrast product solution;

The preparation of need testing solution: get this product 5 grams, the accurate title, decide, and adds methanol 50ml, dissolving, filter, volatilize, be dissolved in water, add water saturated n-butyl alcohol 25ml extraction 5 times, merge n-butanol extracting liquid, add the ammonia solution triplication, shake up, place, divide and get upper solution, evaporate to dryness, residue add methanol makes dissolving, quantitatively moves in the 5ml measuring bottle, add methanol and be diluted to scale, shake up, promptly;

Chromatographic condition: with octadecylsilane chemically bonded silica is filler; Volume ratio is that 99: 400 acetonitrile-0.05% phosphoric acid solution is a mobile phase; Detect wavelength 203nm;

Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject hplc determination;

(2) assay method of astragaloside is:

Chromatographic condition: octadecylsilane chemically bonded silica is a filler; Evaporative light scattering detector;

Mobile phase: ratio is acetonitrile-water-oxolane of 33: 67: 4;

The preparation of reference substance solution: get the astragaloside reference substance and add methanol and make the solution that every 1ml contains 0.5mg, shake up;

The preparation of need testing solution: get about 3 grams of this product, the accurate title, decide, and adds water 30ml dissolving, filter, filtrate is used defat with petroleum ether 3 times, and water liquid extracts (each 30ml) 5 times with water saturated n-butyl alcohol jolting, merge n-butanol extracting liquid, extract 2 times, each 30ml with ammonia solution, discard ammonia solution, the water 30ml saturated with n-butyl alcohol washes, and discards water liquid, n-butyl alcohol liquid evaporate to dryness, residue adds water 7mL makes dissolving, puts coldly, passes through D ₁₀₁Type macroporous adsorptive resins (internal diameter 1.5cm, long 18cm) is with water elution, discard water liquid, reuse 30% ethanol 60ml eluting discards ethanol elution, continue with 60% ethanol 80ml eluting, collect eluent, evaporate to dryness is with dissolve with methanol and be transferred in the 5ml measuring bottle, add methanol to scale, shake up, filter, promptly.

The result: every gram drop pill contains ginsenoside Re 0.2mg, contains astragaloside 5mg.

Embodiment 6

Ginsenoside 8g Radix Astragali 150g Radix Rehmanniae 250g

Radix Ophiopogonis 80g Radix Trichosanthis 40g Fructus Lycii 160g

Fructus Schisandrae Chinensis 80g Rhizoma Dioscoreae 80g Fructus Rubi 50g

Poria 80g Rhizoma Alismatis 80g

Method for making: a Radix Ophiopogonis is with warm water lixiviate 2 times, and each 2 hours, merge lixiviating solution, filter, it is 1.40 thick paste that filtrate is concentrated into relative density;

B Fructus Schisandrae Chinensis 50% ethanol, percolation, percolate reclaim ethanol, are concentrated into thick paste;

C Fructus Lycii, the Radix Astragali, Radix Rehmanniae, Rhizoma Alismatis, Rhizoma Dioscoreae, Radix Trichosanthis, Fructus Rubi, Poria water decoct 3 times, and each 2 hours, merging decoction liquor, filtration, filtrate, to be concentrated into relative density be 1.20 thick paste, add ethanol and make that to contain the alcohol amount be 70%, leave standstill, the leaching supernatant, reclaim ethanol, concentrate

D merges drying, pulverizing and ginsenoside with above-mentioned extractum and merges, mixing gets extract powder 100g, add the extract powder mixing after getting adjuvant polyethylene glycol 6000 800g, tween 80 100g heating and melting, move in the drop pill machine storage tank, in the water dropper temperature is under 750 ℃ of conditions, splashes in the dimethicone with 130 droplets/minute the speed of dripping, and removes liquid coolant, select ball, promptly.

Content assaying method:

(1) ginsenoside Re's assay method is:

The preparation of reference substance solution: it is an amount of that precision takes by weighing ginsenoside Re's reference substance, adds methanol and make the solution that contains ginsenoside Re 0.4mg among every 1ml respectively, in contrast product solution;

The preparation of need testing solution: get this product 5 grams, the accurate title, decide, and adds methanol 50ml, dissolving, filter, volatilize, be dissolved in water, add water saturated n-butyl alcohol 25ml extraction 5 times, merge n-butanol extracting liquid, add the ammonia solution triplication, shake up, place, divide and get upper solution, evaporate to dryness, residue add methanol makes dissolving, quantitatively moves in the 5ml measuring bottle, add methanol and be diluted to scale, shake up, promptly;

Chromatographic condition: with octadecylsilane chemically bonded silica is filler; Volume ratio is that 99: 400 acetonitrile-0.05% phosphoric acid solution is a mobile phase; Detect wavelength 203nm;

Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject hplc determination;

(2) assay method of astragaloside is:

Chromatographic condition: octadecylsilane chemically bonded silica is a filler; Evaporative light scattering detector;

Mobile phase: ratio is acetonitrile-water-oxolane of 33: 67: 4;

The preparation of reference substance solution: get the astragaloside reference substance and add methanol and make the solution that every 1ml contains 0.5mg, shake up;

The preparation of need testing solution: get about 3 grams of this product, the accurate title, decide, and adds water 30ml dissolving, filter, filtrate is used defat with petroleum ether 3 times, and water liquid extracts (each 30ml) 5 times with water saturated n-butyl alcohol jolting, merge n-butanol extracting liquid, extract 2 times, each 30ml with ammonia solution, discard ammonia solution, the water 30ml saturated with n-butyl alcohol washes, and discards water liquid, n-butyl alcohol liquid evaporate to dryness, residue adds water 7mL makes dissolving, puts coldly, passes through D ₁₀₁Type macroporous adsorptive resins (internal diameter 1.5cm, long 18cm) is with water elution, discard water liquid, reuse 30% ethanol 60ml eluting discards ethanol elution, continue with 60% ethanol 80ml eluting, collect eluent, evaporate to dryness is with dissolve with methanol and be transferred in the 5ml measuring bottle, add methanol to scale, shake up, filter, promptly.

The result: every gram drop pill contains ginsenoside Re 1mg, contains astragaloside 1mg.

Embodiment 7

Ginsenoside 8g Radix Astragali 150g Radix Rehmanniae 250g

Radix Ophiopogonis 80g Radix Trichosanthis 80g Fructus Lycii 80g

Fructus Schisandrae Chinensis 80g Rhizoma Dioscoreae 80g Fructus Rubi 50g

Poria 80g Rhizoma Alismatis 80g

Method for making: a Radix Ophiopogonis is with warm water lixiviate 2 times, and each 2 hours, merge lixiviating solution, filter, it is 1.40 thick paste that filtrate is concentrated into relative density;

B Fructus Schisandrae Chinensis 50% ethanol, percolation, percolate reclaim ethanol, are concentrated into thick paste;

C Fructus Lycii, the Radix Astragali, Radix Rehmanniae, Rhizoma Alismatis, Rhizoma Dioscoreae, Radix Trichosanthis, Fructus Rubi, Poria water decoct 3 times, and each 2 hours, merging decoction liquor, filtration, filtrate, to be concentrated into relative density be 1.20 thick paste, add ethanol and make that to contain the alcohol amount be 70%, leave standstill, the leaching supernatant, reclaim ethanol, concentrate

D merges drying, pulverizing and ginsenoside with above-mentioned extractum and merges, mixing gets extract powder 100g, add the extract powder mixing after getting adjuvant Macrogol 4000 100g, polyethylene glycol 6000 200g heating and melting, move in the drop pill machine storage tank, in the water dropper temperature is under 75 ℃ of conditions, splashes in the liquid coolant dimethicone with 80 droplets/minute the speed of dripping, and removes liquid coolant, select ball, promptly.

Content assaying method: with embodiment 4

The result: every gram drop pill contains ginsenoside Re 1mg, contains astragaloside 0.1mg.

Embodiment 8

Ginsenoside 8g Radix Astragali 150g Radix Rehmanniae 250g

Radix Ophiopogonis 80g Radix Trichosanthis 80g Fructus Lycii 160g

Fructus Schisandrae Chinensis 40g Rhizoma Dioscoreae 80g Fructus Rubi 50g

Poria 80g Rhizoma Alismatis 80g

Method for making: a Radix Ophiopogonis is with warm water lixiviate 2 times, and each 2 hours, merge lixiviating solution, filter, it is 1.40 thick paste that filtrate is concentrated into relative density;

B Fructus Schisandrae Chinensis 50% ethanol, percolation, percolate reclaim ethanol, are concentrated into thick paste;

C Fructus Lycii, the Radix Astragali, Radix Rehmanniae, Rhizoma Alismatis, Rhizoma Dioscoreae, Radix Trichosanthis, Fructus Rubi, Poria water decoct 3 times, and each 2 hours, merging decoction liquor, filtration, filtrate, to be concentrated into relative density be 1.20 thick paste, add ethanol and make that to contain the alcohol amount be 70%, leave standstill, the leaching supernatant, reclaim ethanol, concentrate

D merges drying, pulverizing and ginsenoside with above-mentioned extractum and merges, mixing gets extract powder 100g, add the extract powder mixing after getting adjuvant polyethylene glycol 6000 300g, glycerin gelatine 200g heating and melting, move in the drop pill machine storage tank, in the water dropper temperature is under 75 ℃ of conditions, splashes in the liquid coolant dimethicone with 100 droplets/minute the speed of dripping, and removes liquid coolant, select ball, promptly.

Content assaying method: with embodiment 5

The result: every gram drop pill contains ginsenoside Re 10mg, contains astragaloside 0.4mg.

Embodiment 9

Ginsenoside 8g Radix Astragali 150g Radix Rehmanniae 250g

Radix Ophiopogonis 80g Radix Trichosanthis 80g Fructus Lycii 160g

Fructus Schisandrae Chinensis 80g Rhizoma Dioscoreae 40g Fructus Rubi 50g

Poria 80g Rhizoma Alismatis 80g

Method for making: a Radix Ophiopogonis is with warm water lixiviate 2 times, and each 2 hours, merge lixiviating solution, filter, it is 1.30 thick paste that filtrate is concentrated into relative density;

B Fructus Schisandrae Chinensis 50% ethanol, percolation, percolate reclaim ethanol, are concentrated into thick paste;

C Fructus Lycii, the Radix Astragali, Radix Rehmanniae, Rhizoma Alismatis, Rhizoma Dioscoreae, Radix Trichosanthis, Fructus Rubi, Poria water decoct 3 times, and each 2 hours, merging decoction liquor, filtration, filtrate, to be concentrated into relative density be 1.20 thick paste, add ethanol and make that to contain the alcohol amount be 60%, leave standstill, the leaching supernatant, reclaim ethanol, concentrate

D merges drying, pulverizing and ginsenoside with above-mentioned extractum and merges, mixing gets extract powder 100g, add the extract powder mixing after getting adjuvant polyethylene glycol 6000 300g, soft phosphatidase 12 00g heating and melting, move in the drop pill machine storage tank, in the water dropper temperature is under 80 ℃ of conditions, splashes in the liquid coolant liquid paraffin with 100 droplets/minute the speed of dripping, and removes liquid coolant, select ball, promptly.

Content assaying method: with embodiment 3

The result: every gram drop pill contains ginsenoside Re 0.5mg, contains astragaloside 0.1mg.

Embodiment 10

Ginsenoside 8g Radix Astragali 150g Radix Rehmanniae 250g

Radix Ophiopogonis 80g Radix Trichosanthis 80g Fructus Lycii 160g

Fructus Schisandrae Chinensis 80g Rhizoma Dioscoreae 80g Fructus Rubi 20g

Poria 80g Rhizoma Alismatis 80g

Method for making: a Radix Ophiopogonis is with warm water lixiviate 2 times, and each 2 hours, merge lixiviating solution, filter, it is 1.30 thick paste that filtrate is concentrated into relative density;

B Fructus Schisandrae Chinensis 50% ethanol, percolation, percolate reclaim ethanol, are concentrated into thick paste;

C Fructus Lycii, the Radix Astragali, Radix Rehmanniae, Rhizoma Alismatis, Rhizoma Dioscoreae, Radix Trichosanthis, Fructus Rubi, Poria water decoct 3 times, and each 2 hours, merging decoction liquor, filtration, filtrate, to be concentrated into relative density be 1.20 thick paste, add ethanol and make that to contain the alcohol amount be 60%, leave standstill, the leaching supernatant, reclaim ethanol, concentrate

D merges drying, pulverizing and ginsenoside with above-mentioned extractum and merges, mixing gets extract powder 100g, add the extract powder mixing after getting adjuvant polyethylene glycol 6000 300g, soft phosphatidase 12 00g heating and melting, move in the drop pill machine storage tank, in the water dropper temperature is under 80 ℃ of conditions, splashes in the liquid coolant liquid paraffin with 100 droplets/minute the speed of dripping, and removes liquid coolant, select ball, promptly.

Content assaying method: with embodiment 4

The result: every gram drop pill contains ginsenoside Re 15mg, contains astragaloside 0.05mg.

Embodiment 11

Ginsenoside 8g Radix Astragali 150g Radix Rehmanniae 250g

Radix Ophiopogonis 80g Radix Trichosanthis 80g Fructus Lycii 160g

Fructus Schisandrae Chinensis 80g Rhizoma Dioscoreae 80g Fructus Rubi 50g

Poria 40g Rhizoma Alismatis 80g

Method for making: a Radix Ophiopogonis is with warm water lixiviate 2 times, and each 2 hours, merge lixiviating solution, filter, it is 1.30 thick paste that filtrate is concentrated into relative density;

B Fructus Schisandrae Chinensis 50% ethanol, percolation, percolate reclaim ethanol, are concentrated into thick paste;

C Fructus Lycii, the Radix Astragali, Radix Rehmanniae, Rhizoma Alismatis, Rhizoma Dioscoreae, Radix Trichosanthis, Fructus Rubi, Poria water decoct 3 times, and each 2 hours, merging decoction liquor, filtration, filtrate, to be concentrated into relative density be 1.20 thick paste, add ethanol and make that to contain the alcohol amount be 60%, leave standstill, the leaching supernatant, reclaim ethanol, concentrate

D merges drying, pulverizing and ginsenoside with above-mentioned extractum and merges, mixing gets extract powder 100g, add the extract powder mixing after getting adjuvant polyethylene glycol 6000 300g, soft phosphatidase 12 00g heating and melting, move in the drop pill machine storage tank, in the water dropper temperature is under 80 ℃ of conditions, splashes in the liquid coolant liquid paraffin with 100 droplets/minute the speed of dripping, and removes liquid coolant, select ball, promptly.

Content assaying method: with embodiment 3

The result: every gram drop pill contains ginsenoside Re 10mg, contains astragaloside 0.5mg.

Embodiment 12

Ginsenoside 8g Radix Astragali 150g Radix Rehmanniae 250g

Radix Ophiopogonis 80g Radix Trichosanthis 80g Fructus Lycii 160g

Fructus Schisandrae Chinensis 80g Rhizoma Dioscoreae 80g Fructus Rubi 50g

Poria 80g Rhizoma Alismatis 40g.

Method for making: a Radix Ophiopogonis is with warm water lixiviate 2 times, and each 2 hours, merge lixiviating solution, filter, it is 1.30 thick paste that filtrate is concentrated into relative density;

B Fructus Schisandrae Chinensis 50% ethanol, percolation, percolate reclaim ethanol, are concentrated into thick paste;

C Fructus Lycii, the Radix Astragali, Radix Rehmanniae, Rhizoma Alismatis, Rhizoma Dioscoreae, Radix Trichosanthis, Fructus Rubi, Poria water decoct 3 times, and each 2 hours, merging decoction liquor, filtration, filtrate, to be concentrated into relative density be 1.20 thick paste, add ethanol and make that to contain the alcohol amount be 60%, leave standstill, the leaching supernatant, reclaim ethanol, concentrate

D merges drying, pulverizing and ginsenoside with above-mentioned extractum and merges, mixing gets extract powder 100g, add the extract powder mixing after getting adjuvant polyethylene glycol 6000 300g, soft phosphatidase 12 00g heating and melting, move in the drop pill machine storage tank, in the water dropper temperature is under 80 ℃ of conditions, splashes in the liquid coolant liquid paraffin with 100 droplets/minute the speed of dripping, and removes liquid coolant, select ball, promptly.

Content assaying method: with embodiment 3

The result: every gram drop pill contains ginsenoside Re 10mg, contains astragaloside 0.5mg.

Claims (12)

1, a kind of ginseng and astragalis blood glucose loucring dorpping pill is characterized in that it is prepared from as raw materials of effective components by following:

Ginsenoside 4-8 weight portion Radix Astragali 80-150 weight portion Radix Rehmanniae 150-250 weight portion

Radix Ophiopogonis 45-80 weight portion Radix Trichosanthis 40-80 weight portion Fructus Lycii 80-160 weight portion

Fructus Schisandrae Chinensis 40-80 weight portion Rhizoma Dioscoreae 40-80 weight portion Fructus Rubi 20-50 weight portion

Poria 40-80 weight portion Rhizoma Alismatis 40-80 weight portion.

2, drop pill as claimed in claim 1 is characterized in that being prepared from as raw materials of effective components by following:

Ginsenoside's 6 weight portion Radixs Astragali 124 weight portion Radix Rehmanniae 186 weight portions

Radix Ophiopogonis 62 weight portion Radix Trichosanthis, 62 weight portion Fructus Lyciis, 124 weight portions

Fructus Schisandrae Chinensis 62 weight portion Rhizoma Dioscoreaes 62 weight portion Fructus Rubies 31 weight portions

Poria 62 weight portion Rhizoma Alismatis 62 weight portions.

3, as drop pill as described in the claim 1,2, it is characterized in that raw material is extract obtained and be: 1: 1-1: 10 with the Polyethylene Glycol weight ratio.

4,, it is characterized in that formerly extract obtainedly being: 1: 2-1: 5 with the Polyethylene Glycol weight ratio as drop pill as described in the claim 1,2.

5,, it is characterized in that Polyethylene Glycol is the mixture of polyethylene glycol 6000 or polyethylene glycol 6000 and Macrogol 4000 as the described adjuvant of claim 1-3.

6, as the described adjuvant of claim 1-3, the weight ratio that it is characterized in that Macrogol 4000 and polyethylene glycol 6000 is 1: 1-1: 5.

7,, it is characterized in that its adjuvant also can add tween, soft phospholipid or glycerin gelatine except that Polyethylene Glycol as the described drop pill of claim 1-6.

8,, it is characterized in that every drop pill is heavy: 30-100mg as the described drop pill of claim 1-7.

9,, it is characterized in that every gram drop pill contains ginsenoside Re 0.2-20mg as the described drop pill of claim 1-8.

10,, it is characterized in that every gram drop pill contains astragaloside 0.04-5mg as the described drop pill of claim 1-8.

11,, it is characterized in that assay method is as claim 9 and 10 described effective ingredient:

(1) ginsenoside Re's assay method is:

The preparation of reference substance solution: it is an amount of that precision takes by weighing ginsenoside Re's reference substance, adds methanol and make the solution that contains ginsenoside Re 0.2-0.8mg among every 1ml, in contrast product solution;

The preparation of need testing solution: get this product 1-10 gram, the accurate title, decide, and adds methanol 10-50ml, dissolving, filter, volatilize, be dissolved in water, add water saturated n-butyl alcohol 25-100ml extraction 2-6 time, merge n-butanol extracting liquid, add the ammonia solution triplication, shake up, place, divide and get upper solution, evaporate to dryness, residue add methanol makes dissolving, quantitatively moves in the 2-10ml measuring bottle, add methanol and be diluted to scale, shake up, promptly;

Chromatographic condition: with octadecylsilane chemically bonded silica is filler; Volume ratio is that 99: 400 acetonitrile-0.05% phosphoric acid solution is a mobile phase; Detect wavelength 203nm;

Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject hplc determination;

(2) assay method of astragaloside is:

Chromatographic condition: octadecylsilane chemically bonded silica is a filler; Evaporative light scattering detector;

Mobile phase: ratio is acetonitrile-water-oxolane of 33: 67: 4;

The preparation of reference substance solution: get the astragaloside reference substance and add methanol and make the solution that every 1ml contains 0.1-2mg, shake up;

The preparation of need testing solution: get the about 1-5 gram of this product, the accurate title, decide, and adds water 10-50ml dissolving, filter, filtrate is used defat with petroleum ether 1-3 time, and water liquid extracts (each 10-50ml) 2-6 time with water saturated n-butyl alcohol jolting, merge n-butanol extracting liquid, extract 1-2 time, each 5-40ml with ammonia solution, discard ammonia solution, n-butyl alcohol liquid is washed with the saturated water 10-40ml of n-butyl alcohol, discards water liquid, n-butyl alcohol liquid evaporate to dryness, residue adds water 5-10ml makes dissolving, puts coldly, passes through D ₁₀₁Type macroporous adsorptive resins (internal diameter 1.5cm, long 18cm) is with water elution, discard water liquid, reuse 10-40% ethanol 10-100ml eluting discards ethanol elution, continue with 50-90% ethanol 50-150ml eluting, collect eluent, evaporate to dryness is with dissolve with methanol and be transferred in the 2-10ml measuring bottle, add methanol to scale, shake up, filter, promptly.

12, a kind of Chinese medicine dripping pills for the treatment of diabetes is characterized in that being prepared by following steps:

A uses warm water lixiviate 1-3 time Radix Ophiopogonis, and each 0.5-3 hour, merge lixiviating solution, filter, filtrate is condensed into the thick paste that relative density is 1.03-1.40;

The b Fructus Schisandrae Chinensis reclaims ethanol with the ethanol of 40-70%, percolation, percolate, is condensed into thick paste;

C Fructus Lycii, the Radix Astragali, Radix Rehmanniae, Rhizoma Alismatis, Rhizoma Dioscoreae, Radix Trichosanthis, Fructus Rubi, Poria water decoct 1-4 time, each 0.5-3 hour, merging decoction liquor, filtration, filtrate, to be concentrated into relative density be 1.20 thick paste, adding ethanol makes and contains the alcohol amount and be 40%-80%, leave standstill, the leaching supernatant, reclaim ethanol, concentrate;

D merges drying, pulverizing and ginsenoside with above-mentioned extractum and merges, mixing, add the extract powder mixing after getting adjuvant Polyethylene Glycol heating and melting, move in the drop pill machine storage tank, in the water dropper temperature is under the 70-90 ℃ of condition, with 60-150 drip/minute the speed of dripping splash in liquid paraffin or the dimethicone, remove liquid coolant, select ball, promptly.