CN103690606A - Chinese medicinal composition for treating lumbar disc herniation - Google Patents
Chinese medicinal composition for treating lumbar disc herniation Download PDFInfo
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Abstract
The invention provides a Chinese medicinal composition for treating lumbar disc herniation, which is simple to take, short in treatment cycle, high in cure rate and stable in curative effect without a toxic or side effect. The invention also provides a detection method of the Chinese medicinal composition, and the detection method is specifically used for identifying semen strychni, ephedra, red peony root, licorice, Chinese pyrola herb and ligusticum wallichii in the medicinal preparation disclosed by the invention, and determining the contents of ephedrine and strychnine in the medicinal preparation. The detection method is good in repeatability, convenient in operation and favorable for controlling the quality of the composition.
Description
Technical field
The present invention relates to a kind of detection method of Chinese patent medicine, particularly relate to a kind of detection method for the treatment of the Chinese medicine composition of prolapse of lumbar intervertebral disc, belong to field of medicaments.
Background technology
Prolapse of lumbar intervertebral disc, claim again the Annulus Fibrosus of Lumbar Intervertebral Discs disease of breaking, or lumbar intervertebral disc core herniation, it is that after Anular disruption, vertebral pulp is given prominence to a kind of commonly encountered diseases of oppressing spinal nerve root and causing lumbago and skelalgia, be mainly in prime of life physical labourer, man is more than female, and its clinical symptoms cardinal symptom shows: waist, buttocks, thigh and calf are so that the discomforts such as the acid of foot repeated relapsing is swollen, fiber crops pain can occur the symptoms such as amyotrophy when serious.The Therapeutic Method of prolapse of lumbar intervertebral disc mainly contains two kinds of expectant treatment and operative treatments: generally fall ill initially except some special circumstances, all take expectant treatment, comprise waist physiotherapy, traction, oral antiinflammation pain-stopping pharmaceutical, injection glucocorticoid, massage etc.; If more than expectant treatment 3-6 month, symptom, without alleviating or recidivist again, can consider to adopt operative treatment, comprises resection of nucleus pulposus and report of nucleoplasty.The normal traditional therapy adopting of China's traditional Chinese medical science comprises that oral traditional Chinese medicine decoction, the external application of Chinese medicine add massage.But these Therapeutic Method exist that the course for the treatment of is long, cure rate is low (15%-30%) mostly, easily recurrence, medical expense high-technology defect.
The confirmed good recipe > > JIUFEN POWDER of the < < of Qing Dynasty first aid is Semen Strychni (processed), Herba Ephedrae, Olibanum, Myrrha.Clinical practice shows that the party has good therapeutical effect to prolapse of lumbar intervertebral disc.But through us, study discovery, existing preparation exists detection method to fall behind, the uppity shortcoming of product quality.
Summary of the invention
The invention provides a kind of take simple, treatment cycle is short, cure rate is high, the medicine of efficacy consolidation, the treatment prolapse of lumbar intervertebral disc that has no side effect.Its detection method is also provided.
Compositions of the present invention is to be made by the raw material of Chinese medicine of following weight portion:
Cortex araliae chinensis 85-95 part, Herba Erodii 35-45 part, Semen Strychni (processed) 1-3 part,
Herba Pyrolae 35-45 part, Radix Paeoniae Rubra 35-45 part, Cortex Eucommiae 40-52 part,
Herba Ephedrae 25-35 part, Rhizoma Chuanxiong 25-35 part, Radix Glycyrrhizae 15-25 part,
Olibanum 1-3 part, Myrrha (processed) 1-3 part;
For effective control for product quality, we have set up the detection method method of this compositions, the method adopts thin layer chromatography to differentiate Semen Strychni, Herba Ephedrae, Radix Paeoniae Rubra, Radix Glycyrrhizae, Herba Pyrolae, Rhizoma Chuanxiong, adopts high performance liquid chromatography to carry out assay to strychnine, ephedrine composition.This detection method precision, sensitivity and stability are all good, guarantee " safety, the homogeneous, stable, effective, controlled of product quality.”
Dosage form of the present invention can comprise the oral formulations such as tablet, capsule, micropill, drop pill or granule.
Compositions of the present invention is preferably made by the raw material of Chinese medicine of following weight portion:
90 parts of Cortex araliae chinensis, 40 parts of Herba Erodiis, 2 parts of Semen Strychni (processed)s,
Compositions of the present invention is most preferably comprised of the raw material of Chinese medicine of following weight portion:
90 parts of Cortex araliae chinensis, 40 parts of Herba Erodiis, 2 parts of Semen Strychni (processed)s,
40 parts of Herba Pyrolaes, 40 parts of Radix Paeoniae Rubra, 46 parts of the Cortexs Eucommiae,
30 parts, Herba Ephedrae, 30 parts of Rhizoma Chuanxiongs, 20 parts, Radix Glycyrrhizae,
2 parts of Olibanums, 2 parts of Myrrha (processed);
The preparation method of Chinese medicine composition of the present invention can adopt following methods:
Raw material of Chinese medicine by above-mentioned formula is processed through extraction or other modes, make pharmaceutically active substance, subsequently, take this material as raw material, while needing, add medicine acceptable carrier, according to routine techniques granulation, tablet, capsule, micropill or the drop pill of galenic pharmacy.Described active substance can obtain by being selected from the method for following mode, as; By pulverizing, squeeze, calcine, grind, sieve, percolation, extraction, water extraction, alcohol extraction, ester carry, the method such as ketone is carried, chromatography obtains, these active substances can be the materials of extractum form, can be that dry extract can be also fluid extract, can also be high-purity extract, according to the difference of preparation, need to determine to make different concentration.
A kind of preparation method of the present invention is can be according to following step: all medical materials add the water that medical material gross weight 5-10 doubly measures, soak after 1-2 hour, decoct 2-4 time, each 1-2 hour, merging filtrate, relative density 1.15-1.25 while being evaporated to 50～60 ℃, adds ethanol and stirs evenly, and makes medicinal liquid contain alcohol amount and reaches 50-70%, standing, filter, decompression filtrate recycling ethanol relative density 1.20-1.30 while continuing to be concentrated into 50～60 ℃, make the active component of medicine of the present invention.
Another kind of preparation method of the present invention is directly to pulverize each material medicine, adds after a certain amount of starch, pours into capsule.
Chinese medicine composition of the present invention is comprised of above-mentioned 11 taste raw material of Chinese medicine.
Chinese medicine composition of the present invention can add medicine acceptable carrier as required when making preparation, and these carriers can be any carriers that is applicable to making compositions.
For its feature and formula of the present invention, we provide following detection method:
Detection method of the present invention comprises the following steps:
Character is observed, and official method checks content, and content Semen Strychni, Herba Ephedrae, Radix Paeoniae Rubra, Radix Glycyrrhizae, Herba Pyrolae, Rhizoma Chuanxiong are differentiated, the strychnine containing, ephedrine composition are carried out to assay.
Therefore, detection method of the present invention comprises the following steps:
A. the Semen Strychni in pharmaceutical preparation of the present invention, Herba Ephedrae, Radix Paeoniae Rubra, Radix Glycyrrhizae, Herba Pyrolae, Rhizoma Chuanxiong are differentiated;
B. measure the content of pharmaceutical preparation Ephedrine of the present invention and strychnine;
The concrete steps that wherein A differentiates are as follows:
(1) get this product content 2g, porphyrize, hydro-oxidation sodium test solution 10ml makes to dissolve, place 10 minutes, add ether 20ml, supersound process 10 minutes, let cool, divide and get ether layer, filter, get subsequent filtrate 10ml, put water bath method, residue adds dissolve with methanol, filter, filtrate is as need testing solution, separately get strychnine reference substance, add methanol and make every 1ml containing the solution of 0.1mg, product solution in contrast, according to thin layer chromatography (VIB of < < Chinese Pharmacopoeia > > version in 2010), test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel thin-layer plate, the Methanol-water (10: 1) of take is developing solvent, launch, take out, dry, spray is with rare bismuth potassium iodide test solution, in test sample chromatograph, with the corresponding position of reference substance chromatograph on, the speckle that should show same color,
(2) get this product granule 2g, porphyrize, add 0.5mol/L sodium hydroxide test solution 50ml, shake loose, add sodium chloride 5g, supersound process 10 minutes, distillation, with the 100ml measuring bottle that fills the hydrochloric acid solution 5ml of 0.5mol/L, receive to nearly 100ml, shake up, as test solution, separately getting ephedrine hydrochloride reference substance adds methanol and makes every 1ml containing the solution of 0.1mg, product solution in contrast, according to thin layer chromatography, test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel thin-layer plate, the Methanol-water (15: 1) of take is developing solvent, launch, take out, dry, spray is with ninhydrin solution, at 105 ℃, be heated to speckle colour developing clear, in test sample chromatograph, with the corresponding position of reference substance chromatograph on, aobvious identical punctation,
(3) get this product content 2g, porphyrize, 50ml adds diethyl ether, reflux 60 minutes, filter, filtrate collection is standby, medicinal residues volatilize ether, add chloroform 50ml, reflux 3 hours, filter, filtrate evaporate to dryness, residue adds water 5ml to be made to dissolve, be added on weak cation exchange resin post, use 50ml water elution, eluent evaporate to dryness, residue adds acetone 20ml to be made to dissolve, add the active carbon filtration of decolouring in right amount, filtrate is concentrated into about 5ml as need testing solution, separately get peoniflorin reference substance, add acetone and make every 1ml containing the solution of 0.1mg, product solution in contrast, according to thin layer chromatography, test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel thin-layer plate, methanol-the chloroform (10: 1) of take is developing solvent, under ammonia saturated with vapor, launch, take out, dry, spray is with 10% vanillin sulfuric acid solution, in 105 ℃ of heating, make speckle colour developing clear, in test sample chromatograph, with the corresponding position of reference substance chromatograph on, aobvious identical bluish violet speckle,
(4) get the acetone extract under discriminating (3) item, volatilize acetone, residue adds chloroform 5ml to be made to dissolve, as need testing solution, separately get Rhizoma Chuanxiong control medicinal material 1g, add acetone and make control medicinal material solution by need testing solution method for making, according to thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put on same silica gel thin-layer plate respectively, the methanol-chloroform (5: 1) of take is developing solvent, launches, take out, dry, put under ultra-violet lamp (365nm) and inspect, in test sample chromatograph, with the corresponding position of reference substance chromatograph on, the fluorescence speckle of aobvious same color;
(5) get this product content 2g, add acetone 50ml, water-bath low temperature reflux 3 hours, elimination acetone, medicinal residues volatilize acetone, add ethanol 40ml, heating in water bath refluxes 2 hours, filter, filtrate evaporate to dryness, residue adds water 30ml to be made to dissolve, with water saturated n-butanol extraction 2 times, each 40ml, merge n-butyl alcohol liquid, with the saturated water washing of n-butyl alcohol 3 times, each 40ml, discard water liquid, n-butyl alcohol liquid evaporate to dryness, residue adds ethanol 20ml to be made to dissolve, add active carbon appropriate, shake up, place 30 minutes, filter, filtrate is concentrated into about 10ml, as need testing solution, another extracting liquorice acid mono-ammonium reference substance, add ethanol and make every 1ml containing the solution of 0.2mg, product solution in contrast, according to thin layer chromatography, test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel thin-layer plate, chloroform-formic acid-the glacial acetic acid (15: 1: 1) of take is developing solvent, launch, take out, dry, spray is with 20% ethanol solution of sulfuric acid, at 105 ℃, be heated to speckle colour developing clear, put under ultra-violet lamp (365nm) and inspect, in test sample chromatograph, with the corresponding position of reference substance chromatograph on, the fluorescence speckle of aobvious same color,
6) get this product content 2g, add ethanol 50ml, heating in water bath refluxes 2 hours, filter, in filtrate, add equivalent 10% hydrochloric acid solution, heating in water bath refluxes 3 hours, add the about 20ml of water, boil off ethanol, by ethyl acetate, extract 2 times, each 50ml, merge chloroform liquid, steam to about 20ml, filter, filtrate is as need testing solution, separately get oleanolic acid reference substance, add chloroform and make every 1ml containing the solution of 0.1mg, product solution in contrast, according to thin layer chromatography, test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel thin-layer plate, chloroform-the methanol (10:1) of take is developing solvent, launch, take out, dry, spray is with 20% ethanol solution of sulfuric acid, 100 ℃ to be heated to speckle colour developing clear, in test sample chromatograph, with the corresponding position of reference substance chromatograph on, the speckle of aobvious same color under daylight, the fluorescence speckle of the lower aobvious same color of ultra-violet lamp (365nm),
Wherein the concrete steps of B mensuration content are as follows:
(1) assay of strychnine
Chromatographic condition and system suitability be take silica gel as filler; Cyclohexane extraction-chloroform-absolute methanol-the triethylamine (20:75:5:0.4) of take is mobile phase, and flow velocity is 1.0ml/min; Detection wavelength is 254nm, and number of theoretical plate calculates and should be not less than 2000 by strychnine peak;
The about 20mg of strychnine reference substance is got in the preparation of reference substance solution, accurately weighed, puts in 200ml measuring bottle, adds acetic acid ethyl dissolution and is diluted to scale, shakes up, and makes every lml containing the solution of 0.lmg, shakes up, in contrast product solution;
This product granule 2.0g is got in the preparation of need testing solution, accurately weighed, and hydro-oxidation sodium test solution 15ml makes to dissolve, and places 30 minutes, precision adds ether 50ml, weighed weight, supersound process 30 minutes, let cool, with chloroform, supply the weight of less loss, divide and get ether layer, filter, precision measures subsequent filtrate 10ml, puts water bath method, residue adds ethyl acetate and dissolves, and shifts and be settled to 10ml, shakes up, with microporous filter membrane (0.45 μ m), filter, filtrate is as need testing solution
Algoscopy is accurate reference substance solution and each 10 μ l of need testing solution of drawing respectively, and injection liquid chromatography, measures, and obtains;
(2) assay of ephedrine
Chromatographic condition and system suitability be take octadecylsilane chemically bonded silica as filler; Second eyeball-the water (70:30) of take is mobile phase; Detection wavelength is 280nm, and number of theoretical plate calculates and should be not less than 2000 by ephedrine hydrochloride peak;
It is appropriate that the preparation precision of reference substance solution takes ephedrine hydrochloride reference substance, adds water and make every 1ml containing the solution of 10 μ g, shakes up, precision measures 10ml, puts in 25m1 measuring bottle, adds 2.5% hydrochloric acid solution 2ml, 0.25mol/L sodium hydroxide solution 5m1, shake up, place 60 minutes, with 2.5% hydrochloric acid solution, regulate pH value to neutral, add methanol to scale, shake up, with microporous filter membrane (0.45 μ m), filter, get subsequent filtrate, obtain;
It is tolerant that this product 5 intragranulars are got in the preparation of need testing solution, accurately weighed, porphyrize, precision takes about 0.5g, add 0.5mol/L sodium hydroxide solution 50ml, add sodium chloride 5g, supersound process 10 minutes, distillation, with the 100ml measuring bottle that fills 0.5mol/L hydrochloric acid solution 5ml, receive to nearly 100ml, be diluted with water to scale, shake up, precision measures 10ml, put in 25ml measuring bottle, add 2.5% hydrochloric acid solution 2ml, 0.25mol/L sodium hydroxide solution 5m1, shake up, place 60 minutes, with 2.5mol/L hydrochloric acid solution, regulate pH value to neutral, add methanol to scale, shake up, with microporous filter membrane (0.45 μ m), filter, get subsequent filtrate, obtain, algoscopy is accurate reference substance solution and each 6 μ l of need testing solution of drawing respectively, and injection liquid chromatography, measures, and obtains.
The specific embodiment
Embodiment 1 Chinese medicine composition of the present invention
Cortex araliae chinensis 52.2g, Herba Erodii 23.2g, Semen Strychni (processed) 1.16g,
Herba Pyrolae 23.2g, Radix Paeoniae Rubra 23.2g, the Cortex Eucommiae 26.1 g,
Herba Ephedrae 17.4, Rhizoma Chuanxiong 17.4g, Radix Glycyrrhizae 11.6g,
Olibanum 1.16g, Myrrha (processed) 1.16g;
Above 11 taste medicines, mix above all pulverizing medicinal materials, fine powder, add a certain amount of starch, pour into capsule and get final product.
The clinical observation of embodiment 2 Drug therapy prolapse of lumbar intervertebral disc of the present invention
1, physical data:
Patient's 35 examples, male's 20 examples, women's 15 examples, M-F 4: 3; In age 20-60 year, the mean age is 48 years old; Disease burst person 13 examples, chronic author's 22 examples; The course of disease 6 months is with interior person's 22 examples, 6 months above person's 13 examples; Recidivist's 2 examples after Lumbar Disc; Disease type belongs to cold-dampness type 24 examples, blood stasis type 11 examples; Waist CT shows that extrusion position is in L3,41 examples, and L4,5 16 examples, 8 examples between L5, S1, L3,4 and L4,5 outstanding 2 examples simultaneously, L4,5 and, L5, S1 be outstanding 8 examples simultaneously; CT shows intercalated disc extrusion position side 15 examples of taking back, the side that takes over 11 examples, central type 9 examples, outstanding companion's spinal canal stenosis person 2 examples.
2, diagnostic criteria
Diagnosis of Lumber Disc Prolapse standard (1) has waist trauma history, chronic strain or cold-damp person, and most of patient has chronic back pain history at premorbid.(2) lumbago is to buttocks and lower limb radiation, and when abdominal pressure increases, pain increases the weight of.(3) scoliosis, lumbar vertebra physiology orphan degree disappears or is straight, the other tenderness of diseased region vertebra, and to lower limb radiation, waist limitation of activity.(4) lower limb are got involved, and innervation district skin is felt irritated or blunt, and amyotrophy can appear in course of disease elder, and straight-leg raising test and reinforcement test are positive, and patellar tendon, Achilles tendon reflex weaken or disappear, and the big toe back of the body is stretched, plantar flexion flesh muscular strength weakens.(5) X-ray film inspection, spinal column can lateral bending. and lumbar vertebra physiology prolapse disappears, and pathological interspinal gap can narrow down, neighboring edge vertebral body hyperosteogeny; CT picks up position and the degree that can show that intervertebral is outstanding of looking into. and the visible diseased region of nuclear magnetic resonance, NMR has extrusion phenomenon.
3, Therapeutic Method
The compositions that the method for oral embodiment 1 prepares, 3 times on the 1st, each 12g, boiled water is taken after mixing it with water, and observing 4 weeks is a course for the treatment of.Make efficacy evaluation.During treatment, patient be take and lain up as main, stops waist and bears a heavy burden, partial hot compressing. and after symptom alleviates, actively make waist exercise and two lower limb and replace straight lower limb and be raised to maximum tolerated dose.
4, efficacy assessment standard
Clinical recovery: lumbago and skelalgia disappears, raise >=80 degree of straight lower limb, the extensive recovery operation of energy;
Effective: lumbago and skelalgia obviously alleviates, but still have symptom after overcast and rainy and tired, straight lower limb is raised 60-70 degree, can participate in light work;
Take a turn for the better: lumbago and skelalgia alleviates, waist movable function improves, and straight lower limb improves before raising treatment;
Invalid: after treatment, symptom, sign are without improvement.
5, therapeutic outcome:
This organizes 35 examples, follows the tracks of and treats, result: clinical recovery 14 examples, account for 40% through 4 weeks; Effective 10 examples, account for 28.75%; Effective 9 examples. account for 25.71%; Invalid 2 examples, account for 5.72%.Total effective rate is 94.28%.
CT contrast: after 4 weeks treat, carry out CT contrast. wherein, 14 person's of falling clinical recovery intervertebral disk hernia scopes all have dwindling in various degree, and from 1-15mm, all the other 21 routine CT are shown in that intervertebral disc is without obviously dwindling.
Follow up a case by regular visits to situation: treatment is followed up a case by regular visits to later six months, and 14 routine cured persons are without recurrence; Asymptomatic the increasing the weight of of 10 routine effective person; The .5 example symptom treatment that increases the weight of to transfer from one hospital to another in 9 routine responders, 2 routine nonresponders are row operative treatment.
River, man, 41 years old, on February 26th, 2006, pain, numbness outside lumbago companion right lower extremity, walking disorder.Through CT examination, be 3-4 prolapse of lumbar intervertebral disc, once took meloxicam, bulleyaconitine A sheet, symptom, without after being clearly better, is taken Chinese medicine decoction of the present invention, and serveing on 20 days was 1 course for the treatment of, and lumbago and skelalgia alleviates, and waist movable function improves.Take after 2 courses for the treatment of, sign disappears, and more than straight lower limb is raised 70 degree, can recover normal work.
Zhang, man, 37 years old, on April 13rd, 2009, when readme is worked, the abnormal pain of waist, have a medical check-up: waist limitation of activity, spinal column is lateral bending left, and Western medicine diagnose is prolapse of lumbar intervertebral disc.Serve on 10 days, spiritual amelioration, pain obviously alleviates, and straight lower limb can be raised 50 degree.Follow up a case by regular visits to and within 2 years, have no recurrence.
The detection method of the compositions of embodiment 3, embodiment 1
Described detection method comprises the following steps:
A. the Semen Strychni in pharmaceutical preparation of the present invention, Herba Ephedrae, Radix Paeoniae Rubra, Radix Glycyrrhizae, Herba Pyrolae, Rhizoma Chuanxiong are differentiated;
B. measure the content of pharmaceutical preparation Ephedrine of the present invention and strychnine;
The concrete steps that wherein A differentiates are as follows:
(1) get this product content 2g, porphyrize, hydro-oxidation sodium test solution 10ml makes to dissolve, place 10 minutes, add ether 20ml, supersound process 10 minutes, let cool, divide and get ether layer, filter, get subsequent filtrate 10ml, put water bath method, residue adds dissolve with methanol, filter, filtrate is as need testing solution, separately get strychnine reference substance, add methanol and make every 1ml containing the solution of 0.1mg, product solution in contrast, according to thin layer chromatography (VIB of < < Chinese Pharmacopoeia > > version in 2010), test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel thin-layer plate, the Methanol-water (10: 1) of take is developing solvent, launch, take out, dry, spray is with rare bismuth potassium iodide test solution, in test sample chromatograph, with the corresponding position of reference substance chromatograph on, the speckle that should show same color,
(2) get this product granule 2g, porphyrize, add 0.5mol/L sodium hydroxide test solution 50ml, shake loose, add sodium chloride 5g, supersound process 10 minutes, distillation, with the 100ml measuring bottle that fills the hydrochloric acid solution 5ml of 0.5mol/L, receive to nearly 100ml, shake up, as test solution, separately getting ephedrine hydrochloride reference substance adds methanol and makes every 1ml containing the solution of 0.1mg, product solution in contrast, according to thin layer chromatography, test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel thin-layer plate, the Methanol-water (15: 1) of take is developing solvent, launch, take out, dry, spray is with ninhydrin solution, at 105 ℃, be heated to speckle colour developing clear, in test sample chromatograph, with the corresponding position of reference substance chromatograph on, aobvious identical punctation,
(3) get this product content 2g, porphyrize, 50ml adds diethyl ether, reflux 60 minutes, filter, filtrate collection is standby, medicinal residues volatilize ether, add chloroform 50ml, reflux 3 hours, filter, filtrate evaporate to dryness, residue adds water 5ml to be made to dissolve, be added on weak cation exchange resin post, use 50ml water elution, eluent evaporate to dryness, residue adds acetone 20ml to be made to dissolve, add the active carbon filtration of decolouring in right amount, filtrate is concentrated into about 5ml as need testing solution, separately get peoniflorin reference substance, add acetone and make every 1ml containing the solution of 0.1mg, product solution in contrast, according to thin layer chromatography, test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel thin-layer plate, methanol-the chloroform (10: 1) of take is developing solvent, under ammonia saturated with vapor, launch, take out, dry, spray is with 10% vanillin sulfuric acid solution, in 105 ℃ of heating, make speckle colour developing clear, in test sample chromatograph, with the corresponding position of reference substance chromatograph on, aobvious identical bluish violet speckle,
(4) get the acetone extract under discriminating (3) item, volatilize acetone, residue adds chloroform 5ml to be made to dissolve, as need testing solution, separately get Rhizoma Chuanxiong control medicinal material 1g, add acetone and make control medicinal material solution by need testing solution method for making, according to thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put on same silica gel thin-layer plate respectively, the methanol-chloroform (5: 1) of take is developing solvent, launches, take out, dry, put under ultra-violet lamp (365nm) and inspect, in test sample chromatograph, with the corresponding position of reference substance chromatograph on, the fluorescence speckle of aobvious same color;
(5) get this product content 2g, add acetone 50ml, water-bath low temperature reflux 3 hours, elimination acetone, medicinal residues volatilize acetone, add ethanol 40ml, heating in water bath refluxes 2 hours, filter, filtrate evaporate to dryness, residue adds water 30ml to be made to dissolve, with water saturated n-butanol extraction 2 times, each 40ml, merge n-butyl alcohol liquid, with the saturated water washing of n-butyl alcohol 3 times, each 40ml, discard water liquid, n-butyl alcohol liquid evaporate to dryness, residue adds ethanol 20ml to be made to dissolve, add active carbon appropriate, shake up, place 30 minutes, filter, filtrate is concentrated into about 10ml, as need testing solution, another extracting liquorice acid mono-ammonium reference substance, add ethanol and make every 1ml containing the solution of 0.2mg, product solution in contrast, according to thin layer chromatography, test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel thin-layer plate, chloroform-formic acid-the glacial acetic acid (15: 1: 1) of take is developing solvent, launch, take out, dry, spray is with 20% ethanol solution of sulfuric acid, at 105 ℃, be heated to speckle colour developing clear, put under ultra-violet lamp (365nm) and inspect, in test sample chromatograph, with the corresponding position of reference substance chromatograph on, the fluorescence speckle of aobvious same color,
6) get this product content 2g, add ethanol 50ml, heating in water bath refluxes 2 hours, filter, in filtrate, add equivalent 10% hydrochloric acid solution, heating in water bath refluxes 3 hours, add the about 20ml of water, boil off ethanol, by ethyl acetate, extract 2 times, each 50ml, merge chloroform liquid, steam to about 20ml, filter, filtrate is as need testing solution, separately get oleanolic acid reference substance, add chloroform and make every 1ml containing the solution of 0.1mg, product solution in contrast, according to thin layer chromatography, test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel thin-layer plate, chloroform-the methanol (10:1) of take is developing solvent, launch, take out, dry, spray is with 20% ethanol solution of sulfuric acid, 100 ℃ to be heated to speckle colour developing clear, in test sample chromatograph, with the corresponding position of reference substance chromatograph on, the speckle of aobvious same color under daylight, the fluorescence speckle of the lower aobvious same color of ultra-violet lamp (365nm),
Wherein the concrete steps of B mensuration content are as follows:
(1) assay of strychnine
Chromatographic condition and system suitability be take silica gel as filler; Cyclohexane extraction-chloroform-absolute methanol-the triethylamine (20:75:5:0.4) of take is mobile phase, and flow velocity is 1.0ml/min; Detection wavelength is 254nm, and number of theoretical plate calculates and should be not less than 2000 by strychnine peak;
The about 20mg of strychnine reference substance is got in the preparation of reference substance solution, accurately weighed, puts in 200ml measuring bottle, adds acetic acid ethyl dissolution and is diluted to scale, shakes up, and makes every lml containing the solution of 0.lmg, shakes up, in contrast product solution;
This product granule 2.0g is got in the preparation of need testing solution, accurately weighed, and hydro-oxidation sodium test solution 15ml makes to dissolve, and places 30 minutes, precision adds ether 50ml, weighed weight, supersound process 30 minutes, let cool, with chloroform, supply the weight of less loss, divide and get ether layer, filter, precision measures subsequent filtrate 10ml, puts water bath method, residue adds ethyl acetate and dissolves, and shifts and be settled to 10ml, shakes up, with microporous filter membrane (0.45 μ m), filter, filtrate is as need testing solution
Algoscopy is accurate reference substance solution and each 10 μ l of need testing solution of drawing respectively, and injection liquid chromatography, measures, and obtains;
(2) assay of ephedrine
Chromatographic condition and system suitability be take octadecylsilane chemically bonded silica as filler; Second eyeball-the water (70:30) of take is mobile phase; Detection wavelength is 280nm, and number of theoretical plate calculates and should be not less than 2000 by ephedrine hydrochloride peak;
It is appropriate that the preparation precision of reference substance solution takes ephedrine hydrochloride reference substance, adds water and make every 1ml containing the solution of 10 μ g, shakes up, precision measures 10ml, puts in 25m1 measuring bottle, adds 2.5% hydrochloric acid solution 2ml, 0.25mol/L sodium hydroxide solution 5m1, shake up, place 60 minutes, with 2.5% hydrochloric acid solution, regulate pH value to neutral, add methanol to scale, shake up, with microporous filter membrane (0.45 μ m), filter, get subsequent filtrate, obtain;
It is tolerant that this product 5 intragranulars are got in the preparation of need testing solution, accurately weighed, porphyrize, precision takes about 0.5g, add 0.5mol/L sodium hydroxide solution 50ml, add sodium chloride 5g, supersound process 10 minutes, distillation, with the 100ml measuring bottle that fills 0.5mol/L hydrochloric acid solution 5ml, receive to nearly 100ml, be diluted with water to scale, shake up, precision measures 10ml, put in 25ml measuring bottle, add 2.5% hydrochloric acid solution 2ml, 0.25mol/L sodium hydroxide solution 5m1, shake up, place 60 minutes, with 2.5mol/L hydrochloric acid solution, regulate pH value to neutral, add methanol to scale, shake up, with microporous filter membrane (0.45 μ m), filter, get subsequent filtrate, obtain, algoscopy is accurate reference substance solution and each 6 μ l of need testing solution of drawing respectively, and injection liquid chromatography, measures, and obtains.
Claims (5)
1. treat a Chinese medicine composition for prolapse of lumbar intervertebral disc, it is characterized in that the raw material of Chinese medicine that described compositions comprises following weight portion: Cortex araliae chinensis 85-95 part, Herba Erodii 35-45 part, Semen Strychni (processed) 1-3 part.
2. Chinese medicine composition according to claim 1, it is characterized in that raw material of Chinese medicine: Cortex araliae chinensis 85-95 part that described compositions comprises following weight portion, Herba Erodii 35-45 part, Semen Strychni (processed) 1-3 part, Herba Pyrolae 35-45 part, Radix Paeoniae Rubra 35-45 part, Cortex Eucommiae 40-52 part, Herba Ephedrae 25-35 part, Rhizoma Chuanxiong 25-35 part, Radix Glycyrrhizae 15-25 part, Olibanum 1-3 part, Myrrha (processed) 1-3 part.
3. Chinese medicine composition according to claim 1, it is characterized in that 90 parts of the raw material of Chinese medicine: Cortex araliae chinensis that described compositions comprises following weight portion, 40 parts of Herba Erodiis, 2 parts of Semen Strychni (processed)s, 40 parts of Herba Pyrolaes, 40 parts of Radix Paeoniae Rubra, 46 parts of the Cortexs Eucommiae, 30 parts, Herba Ephedrae, 30 parts of Rhizoma Chuanxiongs, 20 parts, Radix Glycyrrhizae, 2 parts of Olibanums, 2 parts of Myrrha (processed)s.
4. the preparation method of the Chinese medicine composition described in claim 1,2 and 3, is characterized in that: ， is Jiang Cortex araliae chinensis 85-95 part by weight, Herba Erodii 35-45 part, Semen Strychni (processed) 1-3 part, Herba Pyrolae 35-45 part, Radix Paeoniae Rubra 35-45 part, Cortex Eucommiae 40-52 part, Herba Ephedrae 25-35 part, Rhizoma Chuanxiong 25-35 part, Radix Glycyrrhizae 15-25 part, Olibanum 1-3 part, the pulverizing of Myrrha (processed) 1-3 part mixes, add how many parts? starch, pours into capsule, obtains.
5. test right requires a kind of method for the treatment of the Chinese medicine composition of prolapse of lumbar intervertebral disc described in 1,2 and 3, it is characterized in that: comprise the following steps:
A. the Semen Strychni in pharmaceutical preparation of the present invention, Herba Ephedrae, Radix Paeoniae Rubra, Radix Glycyrrhizae, Herba Pyrolae, Rhizoma Chuanxiong are differentiated;
B. measure the content of pharmaceutical preparation Ephedrine of the present invention and strychnine;
The concrete steps that wherein A differentiates are as follows:
1) get this product content 2g, porphyrize, hydro-oxidation sodium test solution 10ml makes to dissolve, place 10 minutes, add ether 20ml, supersound process 10 minutes, let cool, divide and get ether layer, filter, get filtrate 10ml, put water bath method, residue adds dissolve with methanol, filter, filtrate is as need testing solution, separately get strychnine reference substance, add methanol and make every 1ml containing the solution of 0.1mg, product solution in contrast, with reference to the thin layer chromatography test in VIB of < < Chinese Pharmacopoeia > > version in 2010, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel thin-layer plate, the Methanol-water (10: 1) of take is developing solvent, launch, take out, dry, spray is with rare bismuth potassium iodide test solution, in test sample chromatograph, with the corresponding position of reference substance chromatograph on, the speckle that should show same color,
2) get this product granule 2g, porphyrize, add 0.5mol/L sodium hydroxide test solution 50ml, shake loose, add sodium chloride 5g, supersound process 10 minutes, distillation, with the 100ml measuring bottle that fills the hydrochloric acid solution 5ml of 0.5mol/L, receive to nearly 100ml, shake up, as test solution, separately getting ephedrine hydrochloride reference substance adds methanol and makes every 1ml containing the solution of 0.1mg, product solution in contrast, according to thin layer chromatography, test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel thin-layer plate, the Methanol-water (15: 1) of take is developing solvent, launch, take out, dry, spray is with ninhydrin solution, at 105 ℃, be heated to speckle colour developing clear, in test sample chromatograph, with the corresponding position of reference substance chromatograph on, aobvious identical punctation,
3) get this product content 2g, porphyrize, 50ml adds diethyl ether, reflux 60 minutes, filter, filtrate collection is standby, medicinal residues volatilize ether, add chloroform 50ml, reflux 3 hours, filter, filtrate evaporate to dryness, residue adds water 5ml to be made to dissolve, be added on weak cation exchange resin post, use 50ml water elution, eluent evaporate to dryness, residue adds acetone 20ml to be made to dissolve, add the active carbon filtration of decolouring in right amount, filtrate is concentrated into about 5ml as need testing solution, separately get peoniflorin reference substance, add acetone and make every 1ml containing the solution of 0.1mg, product solution in contrast, according to thin layer chromatography, test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel thin-layer plate, methanol-the chloroform (10: 1) of take is developing solvent, under ammonia saturated with vapor, launch, take out, dry, spray is with 10% vanillin sulfuric acid solution, in 105 ℃ of heating, make speckle colour developing clear, in test sample chromatograph, with the corresponding position of reference substance chromatograph on, aobvious identical bluish violet speckle,
4) get A and differentiate 3) in acetone extract, volatilize acetone, residue adds chloroform 5ml to be made to dissolve, as need testing solution, separately get Rhizoma Chuanxiong control medicinal material 1g, add acetone and make control medicinal material solution by need testing solution method for making, according to thin layer chromatography, test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel thin-layer plate, the methanol solution that the volumetric concentration of take is 83.3% is developing solvent, launch, take out, dry, put under ultra-violet lamp 365nm wavelength and inspect, in test sample chromatograph, with the corresponding position of reference substance chromatograph on, the fluorescence speckle of aobvious same color,
5) get this product content 2g, add acetone 50ml, water-bath low temperature reflux 3 hours, elimination acetone, medicinal residues volatilize acetone, add ethanol 40ml, heating in water bath refluxes 2 hours, filter, filtrate evaporate to dryness, residue adds water 30ml to be made to dissolve, with water saturated n-butanol extraction 2 times, each 40ml, merge n-butyl alcohol liquid, with the saturated water washing of n-butyl alcohol 3 times, each 40ml, discard water liquid, n-butyl alcohol liquid evaporate to dryness, residue adds ethanol 20ml to be made to dissolve, add active carbon appropriate, shake up, place 30 minutes, filter, filtrate is concentrated into about 10ml, as need testing solution, another extracting liquorice acid mono-ammonium reference substance, add ethanol and make every 1ml containing the solution of 0.2mg, product solution in contrast, according to thin layer chromatography, test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel thin-layer plate, the chloroform that the volume ratio of take is 15: 1: 1, the mixed liquor of formic acid and glacial acetic acid is developing solvent, launch, take out, dry, spray is with 20% ethanol solution of sulfuric acid, at 105 ℃, be heated to speckle colour developing clear, put under ultra-violet lamp 365nm wavelength and inspect, in test sample chromatograph, with the corresponding position of reference substance chromatograph on, the fluorescence speckle of aobvious same color,
6) get this product content 2g, add ethanol 50ml, heating in water bath refluxes 2 hours, filter, in filtrate, add equivalent 10% hydrochloric acid solution, heating in water bath refluxes 3 hours, add the about 20ml of water, boil off ethanol, by ethyl acetate, extract 2 times, each 50ml, merge chloroform liquid, steam to about 20ml, filter, filtrate is as need testing solution, separately get oleanolic acid reference substance, add chloroform and make every 1ml containing the solution of 0.1mg, product solution in contrast, according to thin layer chromatography, test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel thin-layer plate, the chloroform that the volume ratio of take is 10:1 and the mixed liquor of methanol are developing solvent, launch, take out, dry, spray is with 20% ethanol solution of sulfuric acid, 100 ℃ to be heated to speckle colour developing clear, in test sample chromatograph, with the corresponding position of reference substance chromatograph on, the speckle of aobvious same color under daylight, the fluorescence speckle of aobvious same color under ultra-violet lamp 365nm wavelength,
Wherein the concrete steps of B mensuration content are as follows:
1) assay of strychnine
Chromatographic condition and system suitability be take silica gel as filler; The mixed liquor of cyclohexane extraction, chloroform, absolute methanol and triethylamine that the volume ratio of take is 20:75:5:0.4 is mobile phase, and flow velocity is 1.0ml/min; Detection wavelength is 254nm, and number of theoretical plate calculates and should be not less than 2000 by strychnine peak;
The about 20mg of strychnine reference substance is got in the preparation of reference substance solution, accurately weighed, puts in 200ml measuring bottle, adds acetic acid ethyl dissolution and is diluted to scale, shakes up, and makes every lml containing the solution of 0.lmg, shakes up, in contrast product solution;
This product granule 2.0g is got in the preparation of need testing solution, accurately weighed, and hydro-oxidation sodium test solution 15ml makes to dissolve, place 30 minutes, precision adds ether 50ml, weighed weight, supersound process 30 minutes, lets cool, and supplies the weight of less loss with chloroform, divide and get ether layer, filter, precision measures subsequent filtrate 10ml, put water bath method, residue adds ethyl acetate and dissolves, and shifts and be settled to 10ml, shake up, with 0.45 μ m microporous filter membrane, filter, filtrate is as need testing solution;
Algoscopy is accurate reference substance solution and each 10 μ l of need testing solution of drawing respectively, and injection liquid chromatography, measures, and obtains;
2) assay of ephedrine
Chromatographic condition and system suitability be take octadecylsilane chemically bonded silica as filler; 70% the second eyeball solution of take is mobile phase; Detection wavelength is 280nm, and number of theoretical plate calculates and should be not less than 2000 by ephedrine hydrochloride peak;
It is appropriate that the preparation precision of reference substance solution takes ephedrine hydrochloride reference substance, adds water and make every 1ml containing the solution of 10 μ g, shakes up, precision measures 10ml, puts in 25m1 measuring bottle, adds 2.5% hydrochloric acid solution 2ml, 0.25mol/L sodium hydroxide solution 5m1, shake up, place 60 minutes, with 2.5% hydrochloric acid solution, regulate pH value to neutral, add methanol to scale, shake up, with 0.45 μ m microporous filter membrane, filter, get subsequent filtrate, obtain;
It is tolerant that this product 5 intragranulars are got in the preparation of need testing solution, accurately weighed, porphyrize, precision takes about 0.5g, add 0.5mol/L sodium hydroxide solution 50ml, add sodium chloride 5g, supersound process 10 minutes, distillation, with the 100ml measuring bottle that fills 0.5mol/L hydrochloric acid solution 5ml, receive to nearly 100ml, be diluted with water to scale, shake up, precision measures 10ml, put in 25ml measuring bottle, add 2.5% hydrochloric acid solution 2ml, 0.25mol/L sodium hydroxide solution 5m1, shake up, place 60 minutes, with 2.5mol/L hydrochloric acid solution, regulate pH value to neutral, add methanol to scale, shake up, 0.45 μ m filters with microporous filter membrane, get filtrate as need testing solution,
Algoscopy is accurate reference substance solution and each 6 μ l of need testing solution of drawing respectively, and injection liquid chromatography, measures, and obtains.
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