CN103743692A - Rapid screening method for illegally added chemicals in small meridian-activating pills - Google Patents
Rapid screening method for illegally added chemicals in small meridian-activating pills Download PDFInfo
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- CN103743692A CN103743692A CN201410041883.0A CN201410041883A CN103743692A CN 103743692 A CN103743692 A CN 103743692A CN 201410041883 A CN201410041883 A CN 201410041883A CN 103743692 A CN103743692 A CN 103743692A
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Abstract
The invention relates to a rapid screening method for illegally added chemicals in small meridian-activating pills. The method comprises the following steps: first, preparing reference substances and test solutions, then, respectively absorbing the reference substance solutions and the test solutions, dipping the reference substance solutions and the test solutions on the same silica gel thin-layer plate, developing up the silica gel thin-layer plate via developing agents, taking out the silica gel thin-layer plate to air, putting the silica gel thin-layer plate under an ultraviolet lamp to observe thin-layer chromatography, spraying sulfuric acid ethanol solutions, putting the silica gel thin-layer plate in an oven for constant temperature heating until the color development of spots on the thin-layer plate is clear, putting the silica gel thin-layer plate under sunlight to observe the thin-layer chromatography, and judging that the result of samples is positive if fluorescence quenching spots or spots in the same color appear simultaneously on the same RF value as the reference substances. Obviously, the method is simple and rapid to operate and low in cost; the problem of the interference of false positive is solved, and high expense and a lot of time caused by adopting the traditional infrared spectroscopy, HPLC-MS (high performance liquid chromatography-mass spectrometry) and the like to determine the illegally added chemicals are avoided, which make effectively monitoring whether chemicals are illegally added to the small meridian-activating pills of Chinese patent medicine possible.
Description
Technical field
The present invention relates to traditional Chinese medicine quality detection field, be specifically related to the illegal quick screening method that adds chemical composition in a kind of Small Meridian-Activating Pill.
Background technology
Small Meridian-Activating Pill is by arisaema cum bile, aconiti preparata,radix, wild aconite root, earthworm, frankincense (system), myrrh (system) Chinese medicine preparation that the totally 6 taste prepared slices of Chinese crude drugs form.Main effect is expelling wind and clearing away cold, the dehumidifying of reducing phlegm, promoting blood circulation and stopping pain.For the numbness disease due to wind-cold damp pathogen impatency, phlegm stagnation in collateral, disease is seen limbs joint pain, or crymodynia, or shouting pain, or pain night very, joint joint stuffiness, numbness contracture.Its preparation method is that arisaema cum bile, aconiti preparata,radix, wild aconite root, earthworm, frankincense (system), myrrh (system) are ground into respectively to fine powder, sieves, and mixes, and every 100g fine powder adds refined honey 120～130g and makes large honeyed bolus.This Chinese medicine preparation complicated component, the bi Zheng such as the clinical pain in the back that is used for the treatment of rheumatic arthritis, rheumatoid arthritis and caused by hyperosteogeny, skelagia, cervicodynia, brachialgia, sciatica, duodenal stasis etc.Belong to Anti-rheumatism Chinese patent drugs.In order to pursue economic interests, some lawless persons in Small Meridian-Activating Pill illegal add there is antipyretic, anti-inflammatory, the cheap chemical composition of analgesic effect, to reach effective effect fast.And patient too much takes in after these chemical compositions in unwitting situation, can cause great harm to health.
In Anti-rheumatism Chinese patent drugs, the illegal chemical composition of adding mainly contains two large classes: antipyretic-antalgic class and glucocorticoids.At present, detect illegal method of adding chemical composition in Anti-rheumatism Chinese patent drugs and be the universal method that does not limit the concrete kind of Chinese patent drug.This universal method relates to all Anti-rheumatism Chinese patent drugs, and scope is wide, but Anti-rheumatism Chinese patent drugs is of a great variety, and the prescription of each Chinese patent drug is all different, very easily produce false " positive " and disturb, result of determination clearly, therefore universal method only can be accomplished scalping.And due to the interference of false " positive ", the chemical composition detecting only limits in antipyretic-antalgic class or glucocorticoids limited several.As " about the detection method research of undeclared prescription drugs in antirheumatic Chinese medicine preparation " (Asia-Pacific traditional medicine .2010.6(6) such as Zhang He: 31-32) first adopt thin-layered chromatography to carry out scalping, then must further adopt infrared spectrum or high performance liquid chromatography verify to positive wherein again.But due to infrared spectrometer, HPLC-MS, GC-MS instrument costliness, and must be manipulated by technical professional, maintenance cost is also high, cannot realize rapid screening and reach the object of monitoring.Obviously, completely for the illegal number of chemical composition that adds in Small Meridian-Activating Pill, build the method that can carry out rapid screening and be very important.Therefore, for the illegal illegal activities of adding chemical composition in Small Meridian-Activating Pill are effectively controlled, ensure that the people is safe and effective for medication, need badly and set up the illegal quick screening method that adds chemical composition in Small Meridian-Activating Pill.
Summary of the invention
The object of this invention is to provide the illegal quick screening method that adds chemical composition in a kind of Small Meridian-Activating Pill, to overcome the deficiencies in the prior art.
Another object of the present invention is to get rid of Small Meridian-Activating Pill and illegal vacation " positive " interference of adding chemical composition, realizes the rapid screening of multiple illegal interpolation chemical composition, reaches the universal feasible of monitoring.
Small Meridian-Activating Pill is a Chinese medicine preparation, although prescription flavour of a drug are few, chemical composition is very complicated, illegally adds chemical composition in addition, very easily occurs vacation " positive " interference during mensuration.Conventionally false " positive " disturbed and must be adopted infrared spectrometer, HPLC-MS, GC-MS to carry out composition confirmation.Research discovery, because 5 kinds of chemical compositions of required examination in Small Meridian-Activating Pill all have the character that is dissolved in methyl alcohol, and methyl alcohol is low to the refined honey solubleness in large honeyed bolus, therefore utilizes this character, selects methyl alcohol as extracting solvent.Consider that Small Meridian-Activating Pill is large honeyed bolus, if do not disperseed, this extraction solvent cannot penetrate in sample, can not fully extract chemical composition to be measured.Therefore get Small Meridian-Activating Pill one ball (3g), after shredding, add zeyssatite and grind, large honeyed bolus fully can be disperseed.Add again methyl alcohol, sample is all soaked, and adopt ultrasonic processing, effectively these 5 kinds of compositions are extracted.Both can avoid the stripping of refined honey in Small Meridian-Activating Pill, be convenient to point sample, can greatly reduce again the interference of other compositions to mensuration in Small Meridian-Activating Pill.Again because of illegal chemical composition difference in adsorptive power on thin layer plate of adding, then go out in Chinese patent drug Small Meridian-Activating Pill, whether illegally to have added 5 kinds of chemical compositions with developping agent examination.
Quick screening method of the present invention is as follows
(1) preparation of reference substance solution: get respectively prednisolone, hydrocortisone, metacortandracin, Triamcinolone acetonide and the each 10mg of hydrocortisone acetate reference substance, with methyl alcohol 10ml dissolving, make reference substance solution.
(2) preparation of need testing solution: get Small Meridian-Activating Pill 3g, shred, add zeyssatite 2g, grind well, add methyl alcohol, ultrasonic processing, filters, and gets filtrate as need testing solution.
(3) carry out examination mensuration: draw respectively reference substance solution 1 μ l, need testing solution 5 μ l, put in same silica G F
254on thin layer plate, with developping agent ascending development, take out, dry, put observation thin-layer chromatography under ultraviolet lamp (wavelength 254nm), and then spray 10% ethanol solution of sulfuric acid, and it is clear to the spot colour developing on thin layer plate to be placed in 105 ℃ of baking oven heated at constant temperature, then puts under daylight and observe thin-layer chromatography.In the chromatogram of above-mentioned two kinds of view modes, Rf value identical with reference substance place occurs if any fluorescent quenching spot or the spot of same color simultaneously, can judge that sample result is positive.
Above-mentioned developping agent is methenyl choloride-acetone-methyl alcohol-strong ammonia solution=18: 6: 2: 0.1(volume ratio).
The condition of above-mentioned ultrasonic processing is 30 minutes, power 250W, frequency 50kHz.
The method judges sample result from being prepared into of reference substance solution, and overall process only needs 1 hour, and can be at same silica G F
254the product of the multiple producers of examination on thin layer plate.Obviously, the inventive method is easy and simple to handle, fast, cost is low, both solved the problem that vacation " positive " that Small Meridian-Activating Pill patent medicine causes because of complicated component is disturbed, also avoided adopt infrared spectrum, HPLC-MS, GC-MS measure the expensive expense and the plenty of time that produce, are therefore in effective monitoring Chinese patent drug Small Meridian-Activating Pill, whether illegally to add chemical composition to become possibility.
Accompanying drawing explanation
Fig. 1: Small Meridian-Activating Pill of the present invention and prednisolone, hydrocortisone, metacortandracin, Triamcinolone acetonide, the TLC chromatogram of hydrocortisone acetate under ultraviolet lamp (wavelength 254nm) condition; Wherein, 1: the need testing solution of Small Meridian-Activating Pill negative sample; 2: the need testing solution of Small Meridian-Activating Pill positive; 3: reference substance solution (spot a: prednisolone; Spot b: hydrocortisone; Spot c: metacortandracin; Spot d: Triamcinolone acetonide; Spot e: hydrocortisone acetate).
Fig. 2: Small Meridian-Activating Pill of the present invention and prednisolone, hydrocortisone, metacortandracin, Triamcinolone acetonide, the hydrocortisone acetate TLC chromatogram under sunshine condition; Wherein, 1: the need testing solution of Small Meridian-Activating Pill negative sample; 2: the need testing solution of Small Meridian-Activating Pill positive; 3: reference substance solution (spot a: prednisolone; Spot b: hydrocortisone; Spot c: metacortandracin; Spot d: Triamcinolone acetonide; Spot e: hydrocortisone acetate).
The need testing solution of the Small Meridian-Activating Pill negative sample in above-mentioned Fig. 1, Fig. 2 is the need testing solution of not preparing according to the preparation method of need testing solution containing the Small Meridian-Activating Pill sample of prednisolone, hydrocortisone, metacortandracin, Triamcinolone acetonide, hydrocortisone acetate.The need testing solution of Small Meridian-Activating Pill positive is the need testing solution that the Small Meridian-Activating Pill sample that contains prednisolone, hydrocortisone, metacortandracin, Triamcinolone acetonide, hydrocortisone acetate is prepared according to the preparation method of need testing solution.
Embodiment
Provide detailed embodiment below.
The present invention adopts: instrument and reagent: Sartoris BP211D electronic balance; AUTO SCIENCE AS10200BT type ultrasonic cleaner; P/G2007 type constant temperature oven; Thin layer plate: silica G F
254thin layer plate (German MERCK lot number: HX929689 specification: 20 × 20cm); It is pure that reagent is analysis; Prednisolone reference substance (lot number: 100153-201004), hydrocortisone reference substance (lot number: 100152-200206), metacortandracin reference substance (lot number: 100199-201002), Triamcinolone acetonide reference substance (lot number: 100055-201103), hydrocortisone acetate reference substance (lot number: 100013-200607), above reference substance provides by National Institute for Food and Drugs Control; Small Meridian-Activating Pill (sign lot number: 130110,20130715,130401,120801,20121201,120012,2111105).
Chromatographic condition: developping agent: methenyl choloride-acetone-methyl alcohol-strong ammonia solution=18: 6: 2: 0.1 (volume ratio); Unfolding condition: temperature: 23 ℃; Relative humidity: 59%; Exhibition distance: 10cm.
The preparation of reference substance solution: get respectively prednisolone, hydrocortisone, metacortandracin, Triamcinolone acetonide and the each 10mg of hydrocortisone acetate reference substance, with methyl alcohol 10ml dissolving, make reference substance solution.
The preparation of need testing solution: get Small Meridian-Activating Pill finished product 3g, shred, add zeyssatite 2g, grind well, add methyl alcohol 10ml, carry out ultrasonic processing, filter, get filtrate as need testing solution.
Above-mentioned ultrasonic treatment conditions are 30 minutes, power 250W, frequency 50kHz.
Carry out examination mensuration: draw respectively reference substance solution 1 μ l, need testing solution 5 μ l, put in same silica G F
254on thin layer plate, with developping agent ascending development, take out, dry, put observation thin-layer chromatography under ultraviolet lamp (wavelength 254nm), and then spray 10% ethanol solution of sulfuric acid, and it is clear to the spot colour developing on thin layer plate to be placed in 105 ℃ of baking oven heated at constant temperature, then puts under daylight and observe thin-layer chromatography.In the chromatogram of above-mentioned two kinds of view modes, Rf value identical with reference substance place occurs if any fluorescent quenching spot or the spot of same color simultaneously, can judge that sample result is positive.Having detected 5 kinds of chemical compositions is prednisolone, hydrocortisone, metacortandracin, Triamcinolone acetonide and hydrocortisone acetate.Corresponding chromatogram as shown in Figure 1, Figure 2.
Result shows, mixes reference substance good separation, and all the components of Small Meridian-Activating Pill self is noiseless to measuring, and at the identical Rf value of reference substance place, noiseless composition exists test sample.
To sum up, whether the thin-layered chromatography that the present invention sets up can illegally add these 5 kinds of chemical compositions of prednisolone, hydrocortisone, metacortandracin, Triamcinolone acetonide and hydrocortisone acetate in fast detecting Chinese patent drug Small Meridian-Activating Pill, have easy and simple to handle, fast, feature cheaply, can be used as the universal method that Small Meridian-Activating Pill Quality of Chinese Traditional Proprietary Medicine is monitored.
Claims (7)
1. an illegal quick screening method that adds chemical composition in Small Meridian-Activating Pill, is characterized in that preparing first respectively reference substance solution (1) and need testing solution (2), then carries out examination mensuration (3):
(1) preparation of reference substance solution: get respectively prednisolone, hydrocortisone, metacortandracin, Triamcinolone acetonide and the each 10mg of hydrocortisone acetate reference substance, with methyl alcohol 10ml dissolving, make reference substance solution;
(2) preparation of need testing solution: get Small Meridian-Activating Pill one ball, shred, add zeyssatite, grind well, add methyl alcohol, ultrasonic processing, filters, and gets filtrate as need testing solution;
(3) carry out examination mensuration: draw respectively reference substance solution, need testing solution, point sample is in same silica G F
254on thin layer plate, using methenyl choloride-acetone-methyl alcohol-strong ammonia solution as developping agent ascending development, take out, dry, put under ultraviolet lamp 254nm and observe thin-layer chromatography, spray again with 10% ethanol solution of sulfuric acid, and it is clear to the spot colour developing on thin layer plate to be placed in 105 ℃ of baking oven heated at constant temperature, then puts under daylight and observe thin-layer chromatography; If in the chromatogram of above-mentioned two kinds of view modes, Rf value identical with reference substance place has fluorescent quenching spot or the spot of same color to occur simultaneously, can judge that sample result is positive, having detected 5 kinds of chemical compositions is prednisolone, hydrocortisone, metacortandracin, Triamcinolone acetonide and hydrocortisone acetate.
2. quick screening method as claimed in claim 1, the volume ratio that it is characterized in that above-mentioned developping agent methenyl choloride-acetone-methyl alcohol-strong ammonia solution is 18: 6: 2: 0.1.
3. quick screening method as claimed in claim 1, is characterized in that above-mentioned zeyssatite weight is 2g.
4. quick screening method as claimed in claim 1, the methyl alcohol volume that it is characterized in that (2) in the claims 1 is 10ml.
5. quick screening method as claimed in claim 1, the point sample volume that it is characterized in that above-mentioned reference substance solution is 1 μ l.
6. quick screening method as claimed in claim 1, the point sample volume that it is characterized in that above-mentioned need testing solution is 5 μ l.
7. quick screening method as claimed in claim 1, the condition that it is characterized in that above-mentioned ultrasonic processing is 30 minutes, power 250W, frequency 50kHz.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106770230A (en) * | 2016-12-02 | 2017-05-31 | 山东省食品药品检验研究院 | A kind of prednisone acetate method for quick |
| CN106814065A (en) * | 2017-01-18 | 2017-06-09 | 山东省食品药品检验研究院 | A kind of hydrocortisone method for quick |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101762673A (en) * | 2009-12-09 | 2010-06-30 | 中国人民武装警察部队药品仪器检验所 | Method for detection of illegally added chemical in traditional Chinese medicine preparation |
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2014
- 2014-01-28 CN CN201410041883.0A patent/CN103743692A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101762673A (en) * | 2009-12-09 | 2010-06-30 | 中国人民武装警察部队药品仪器检验所 | Method for detection of illegally added chemical in traditional Chinese medicine preparation |
Non-Patent Citations (4)
| Title |
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| 中国药品生物制品检定所: "《抗风湿类中成药中非法添加化学药品补充检验方法》", 7 December 2009, article "抗风湿类中成药中非法添加化学药品补充检验方法", pages: 1-11 * |
| 吴小红: "中成药及保健品非法添加化学药品的检测方法学研究", 《中国优秀硕士学位论文全文数据库 医药卫生科技辑》, no. 4, 15 April 2010 (2010-04-15) * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106770230A (en) * | 2016-12-02 | 2017-05-31 | 山东省食品药品检验研究院 | A kind of prednisone acetate method for quick |
| CN106814065A (en) * | 2017-01-18 | 2017-06-09 | 山东省食品药品检验研究院 | A kind of hydrocortisone method for quick |
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Application publication date: 20140423 |