CN105510327A - Method for identifying traditional Chinese medicine material sulfur residues - Google Patents
Method for identifying traditional Chinese medicine material sulfur residues Download PDFInfo
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Abstract
The invention discloses a method for identifying traditional Chinese medicine material sulfur residues and belongs to the field of analysis and detection of the chemical substance residual quantity. The method includes the following steps that traditional Chinese medicine materials are placed in a flask after being smashed; distilled water is added, and ultrasonic processing is carried out; a hydrochloric acid solution is added; heating is conducted for distillation; fractions are absorbed with a strong base solution; an oxidizing agent is added into an absorbing solution and heated; finally, the absorbing solution is dropwise added into precipitator solutions such as barium nitrate, whether precipitate is generated or not is observed, and whether the sulfur residues are contained in the traditional Chinese medicine materials is identified. The detection limit of the method reaches 1 microgramme/g. By means of the method, the sulfur residues in various traditional Chinese medicine materials can be quickly and effectively identified, and the method has the advantages of being universal, low in cost, easy to operate and easy to popularize.
Description
Technical field
The present invention relates to the authentication method that Chinese crude drug sulphur is residual, be specifically related to oxidation processes that in sample, sulphur is residual and precipitation identification method.
Background technology
The Chinese crude drug treatment technology that sulfur fumigation has developed since being the sixties in last century.The sulphuric dioxide produced in sulfur fumigation process, can accelerate the drying of Chinese crude drug, prevents the mouldy, rotten of Chinese crude drug, and increases the color and luster aesthetic feeling of Chinese crude drug, be therefore widely used in the Habitat producing of several kinds of Chinese medicinal materials.At present, the Chinese crude drug of sulfur fumigation is adopted to comprise: more than the 20 kind of parts of generic medicinal plants such as ginseng, Radix Codonopsis, American Ginseng, the root of Dahurain angelica, Chinese yam, lily, matrimony vine, the Radix Astragali, chrysanthemum, honeysuckle, white fungus.But the experimental results shows, sulphuring can cause Chinese medicine wood property deterioration taste, biological active component loss and sulphite and heavy-metal residual.After being used as medicine, drug effect not only can being caused to decline, also can damage eater's health.Therefore, China's coastal port one deletes the content using sulfur fumigation Chinese crude drug, and has recorded sulfur dioxide residual quantity determination method in Chinese Pharmacopoeia version one in 2010.Be carry out acidolysis distillation to Chinese drugs powder in pharmacopeia, the sulphuric dioxide amidin of spilling absorbs, and demarcates residual sulfur dioxide with iodine solution.
The detection method of Sulphur Dioxide in Chinese Herbal Medicines by Iodine Titration Method comprises fast qualitative qualification and quantitative measurement.Fast qualitative qualification is the method utilizing the relevant physicochemical property of sulphuric dioxide or simple instrument to realize sulphuric dioxide Qualitative Identification, has with low cost, easy advantage intuitively, is suitable for the qualification of batch sample.At present, the rapid identification method of sulphuric dioxide has pH identification method, FTIR spectrum method, improves ancient Cai Shi method and iodine test solution method and the barium chloride precipitation method and (thank Yunlong, Lei Peng, contemporary Chinese medical journal, 2001,11 (7): 95,98; Liu Jingjing, Liu Xiao, Li Songlin etc., Nanjing University of Traditional Chinese Medicine's journal, 2010,26 (5): 356-358; Hao Yanjun, Xu Qiuyang, Sang Yuli etc., CHINA JOURNAL OF CHINESE MATERIA MEDICA, 2012,37 (3): 335-337; Yang Dequan, Yuan Hong, traditional Chinese medicine Leader, 2009,15 (9): 51-52), the kind of authentication method is relatively few, and lacks the Data support of broad spectrum activity.
Summary of the invention
The technical issues that need to address of the present invention are to provide the residual rapid identification method of the sulphur after a kind of sulphuring method process that can be applicable to several kinds of Chinese medicinal materials.The qualification of this authentication method is accurate, directly perceived, simple, and cost is very cheap.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is:
The authentication method that Chinese crude drug sulphur is residual, comprises the following steps:
Step one desampling: get Chinese crude drug, is ground into fine powder; Accurately take Chinese crude drug fine powder 2 ~ 10g and put into flask, add distilled water, ultrasound wave process 5 ~ 15 minutes; Then in bottle, hydrochloric acid solution is added; Flask is connected on distilling apparatus, adds thermal distillation, absorb cut with strong base solution; After distillation terminates, regulate cut solution ph to 6.0 ~ 8.0, obtain solution a;
Step 2 sample oxidation: add oxygenant in solution a, adds thermal response 8 ~ 12 minutes, then concentrates, obtain solution b;
Step 3 sample identification: be added in precipitant solution by solution b, generates if observe precipitation, then contain sulfur dioxide residue in sample, and residual quantity is more than or equal to 1 μ g/g; Otherwise then in sample, sulfur dioxide residual quantity is less than 1 μ g/g.
Further improvement of the present invention is: the granularity of fine powder described in step one is less than 1mm.
Further improvement of the present invention is: in step one, the volume of distilled water is 150mL, vapo(u)rizing temperature is 90 ~ 110 DEG C, ultrasonic treatment time is 10 minutes, the volumetric concentration of used salt acid solution is 1:1, and the consumption of hydrochloric acid solution is 50mL, and strong base solution is sodium hydroxide solution or potassium hydroxide solution, strong base solution concentration is 0.05 ~ 0.2mol/L, and the cut liquor capacity distilled out is 50 ~ 70mL.
Further improvement of the present invention is: oxygenant described in step 2 is hydrogen peroxide or ozone, and the heating reaction time is 10 minutes, and the solution b volume after concentrated in step 2 is 10mL.
Further improvement of the present invention is: precipitation agent described in step 3 is water miscible calcium salt, lead salt or barium salt; The concentration of precipitant solution is 0.1 ~ 10mmol/L, and the consumption of precipitant solution is not more than 10mL.
Further improvement of the present invention is: precipitation agent is any one in calcium nitrate, plumbi nitras, barium nitrate, lime chloride or barium chloride.
Further improvement of the present invention is: the Chinese crude drug fine powder amount in step one is 5g; Vapo(u)rizing temperature is 100 DEG C; Strong base solution is concentration is 0.1mol/L sodium hydroxide solution or potassium hydroxide solution; The liquid volume distilled out is 60mL; In step 2, described oxygenant is hydrogen peroxide; Precipitation agent described in step 3 is barium chloride.
Further improvement of the present invention is: described Chinese crude drug is one or more the combination in ginseng, Radix Codonopsis, American Ginseng, the root of Dahurain angelica, Chinese yam, lily, matrimony vine, the Radix Astragali, chrysanthemum, honeysuckle, white fungus.
Owing to have employed technique scheme, the technical progress that the present invention obtains is:
In the desampling step of method of the present invention, the acidification of Chinese crude drug is with reference to methods known in the art (such as, Chinese Pharmacopoeia version annex in 2010), sulphuric dioxide residual in releasing Chinese medicine material.Be with Chinese Pharmacopoeia difference, first Chinese crude drug fine powder adopted Ultrasonic Cleaning process in aqueous, be beneficial to the infiltration of distilled water centering fine medicinal material powder.Then, heat under acid condition, be beneficial to sulphuric dioxide and overflow from solution.Solution is heated to boiling by the present invention, and on the one hand, sulphuric dioxide solubleness in water is lower at relatively high temperatures, and on the other hand, water vapor can carry sulphuric dioxide and overflow from solution.The sulphuric dioxide overflowed, owing to react with highly basic, generates sulphite, and the element sulphur in the solution a therefore obtained by the method exists with the form of sulphite, and namely in Chinese crude drug, sulphur remains and can change sulphite into, and main chemical reactions is:
SO
2+NaOH→Na
2SO
3
The pH value of solution a controls within certain scope by the present invention, can prevent precipitant solution from generating precipitation of hydroxide in the basic conditions, and disturb qualification result.
In the step of sample oxidation, the sodium sulphite generated has certain reductibility, and the present invention by adding oxygenant in solution, and make inferior sulfate radical change sulfate radical into, main chemical reaction is:
SO
3 2-+H
2O
2→SO
4 2-+H
2O
Of the present invention to cut solution carry out suitable molten contracting be qualification successful important step.By concentrating solution, in solution, the concentration of sulfate ion becomes large, and easier and precipitation agent reacts, and generates and precipitates, and is conducive to the traditional Chinese medicinal material samples identifying low residual amt.
In the step of sample identification, by the solution b of certain volume is dropped to precipitant solution, the sulfate ion obtained by Sulphur Dioxide can with precipitation agent effect, generate macroscopic precipitation, thus reach the object of Rapid identification sulphuric dioxide, main chemical reactions is:
SO
4 2-+Pb
2+→PbSO
4↓
SO
4 2-+Ca
2+→CaSO
4↓
SO
4 2-+Ba
2+→BaSO
4↓
Due to the solubility product (K of barium sulphate
sp=1.1 × 10
-11) very little, when sulfate concentration is very low, still can reacts to generate with barium salt and precipitate.Therefore, this authentication method can sulfur dioxide residue effectively in Identification chinese herbs medicine material.After the concentration of suitable adjustment precipitant solution, the detectability of the method can be made to reach 1 μ g/g, and the solution b by certain volume drops in certain density precipitant solution, generates if observe precipitation, then contain sulfur dioxide residue in sample, residual quantity is more than or equal to 1 μ g/g; Otherwise then in sample, sulfur dioxide residual quantity is less than 1 μ g/g.Therefore method of the present invention is suitable for the Chinese crude drug Quality Detection (in Chinese Pharmacopoeia medicinal material and medicine materical crude slice calibrating general rule regulation Chinese crude drug and medicine materical crude slice, sulfur dioxide residual quantity must not more than 150 μ g/g) of high request.
Method of the present invention has lower detection limit, the required Chinese crude drug amount of detection is less.Method of the present invention can detect the residual sulphur of ten several kinds of Chinese medicinal materials such as ginseng, Radix Codonopsis, American Ginseng, the root of Dahurain angelica, Chinese yam, lily, matrimony vine, the Radix Astragali, chrysanthemum, honeysuckle, white fungus, applied range.Combination of Methods of the present invention is convenient, do not pollute the environment, and the feature of environmental protection is better.Method of the present invention is except the qualification remained for Chinese crude drug sulphur; can also be used in some dried fruits; often can add pyrosulfite in dried fruit as antiseptic, the present invention has the sensitivity of height equally to pyrosulfite, can realize the detection to pyrosulfite.
Accompanying drawing explanation
Fig. 1 is the process flow diagram of embodiments of the present invention;
Fig. 2 is the testing result photo that the inventive method detects that different sulphur remains Chinese yam sample.
Embodiment
The authentication method that Chinese crude drug sulphur is residual, applicable Chinese crude drug is one or more the combination in ginseng, Radix Codonopsis, American Ginseng, the root of Dahurain angelica, Chinese yam, lily, matrimony vine, the Radix Astragali, chrysanthemum, honeysuckle, white fungus.Comprise the following steps:
Step one desampling: get Chinese crude drug, is ground into fine powder, and the granularity (particle diameter) of described fine powder is less than 1mm.Accurately take Chinese crude drug fine powder 2 ~ 10g and put into flask, add 150mL distilled water, ultrasound wave process 5 ~ 15 minutes, is preferably 10 minutes; Then in bottle, add 1:1 (volumetric concentration) hydrochloric acid solution 50mL; Be connected to by flask on distilling apparatus, add thermal distillation, vapo(u)rizing temperature is 90 ~ 110 DEG C, is preferably 100 DEG C, absorbs cut with strong base solution, and strong base solution is sodium hydroxide solution or potassium hydroxide solution, and strong base solution concentration is 0.05 ~ 0.2mol/L; After distillation terminates, regulate cut solution ph to 6.0 ~ 8.0, the liquid volume distilled out is 50 ~ 70mL, obtains solution a.
Step 2 sample oxidation: add oxygenant in solution a, described oxygenant is hydrogen peroxide or ozone, preferred hydrogen peroxide; Add thermal response 8 ~ 12 minutes, be preferably 10 minutes, then concentrate, the sample solution volume after concentrated is 10mL, obtains solution b;
Step 3 sample identification: be added to by solution b in no more than 10mL precipitant solution, described precipitation agent is water miscible calcium salt, lead salt, barium salt; The concentration of precipitant solution is 0.1 ~ 1mmol/L, and generate if observe precipitation, then contain sulfur dioxide residue in sample, residual quantity is more than or equal to 1 μ g/g; Otherwise then in sample, sulfur dioxide residual quantity is less than 1 μ g/g.Described precipitation agent to be preferably in calcium nitrate, plumbi nitras, barium nitrate, lime chloride, barium chloride any one.
Below in conjunction with embodiment, the present invention is described in further details:
In following examples, the fresh sample of Chinese crude drug used is all purchased from the market of farm produce.Chinese crude drug natural drying process is by being positioned over dry ventilation, regular turnover by purchasing Chinese crude drug, and no longer change to Chinese crude drug quality, drying time is 10 days.Chinese crude drug stove drying dry run is by by being purchased Chinese crude drug stove drying after 2 hours, and be positioned over dry ventilation, regular turnover, no longer change to Chinese crude drug quality, drying time is 5 days.Before qualification, traditional Chinese medicinal material samples pulverized respectively, powder particle size is less than 1mm.
Embodiment 1:
Accurately take the Chinese yam fine powder of 5g stove drying drying and natural drying, add in two round-bottomed flasks respectively, then adopt following same method to identify the sulfur content in two kinds of Chinese crude drugs.Add 150mL distilled water, ultrasound wave process 10 minutes.Then in bottle, add 1:1 (volumetric concentration, lower same) hydrochloric acid solution 50mL.Round-bottomed flask is connected distilling apparatus, adds thermal distillation, vapo(u)rizing temperature is 100 DEG C, and cut 0.1mol/L sodium hydroxide solution is collected, and the liquid volume distilled out is 60mL.After distillation terminates, about regulating cut solution ph to 7.In solution, add hydrogen peroxide (volumetric concentration is 30%, lower same) and heat.Solution is concentrated into 10mL, and it is in the 5ml barium chloride solution of 1mmol/L that gained solution drops to concentration.Observe the generation of white precipitate in the Chinese yam powder sample solution of stove drying, qualification result contains sulfur dioxide residue in sample, is greater than 1 μ g/g.The Chinese yam powdered sample of natural drying detects by above-mentioned same method, and the Chinese yam powder sample solution of natural drying is then clarified very much, and qualification result there is not sulfur dioxide residue in sample.Come to the same thing with the present embodiment after adopting other method validation beyond the present invention.
Do not add in the Chinese yam fine powder of natural drying or add quantitative sodium sulphite, test according to the method for the invention, experimental result as shown in Figure 2.There is not muddiness in the Chinese yam sample corresponding solution not adding sodium sulphite, and adds the formation all obviously seeing white precipitate in the sodium sulphite sample corresponding solution of different amount, and experimental result understands, and noiseless.
Embodiment 2:
Accurately take the white fungus fine powder of 2g stove drying drying and natural drying, add in two round-bottomed flasks respectively, then adopt following same method to identify the sulfur content in two kinds of Chinese crude drugs.Add 150mL distilled water, ultrasound wave process 10 minutes.Then in bottle, 1:1 hydrochloric acid solution 50mL is added.Flask is connected distilling apparatus, adds thermal distillation, cut 0.05mol/L potassium hydroxide solution is collected.After distillation terminates, regulate cut solution ph to 6.5.In solution, add hydrogen peroxide (30%) and heat.Solution is concentrated into 10mL, and it is in the 5ml lead nitrate solution of 1mmol/L that gained solution drops to concentration.Observe the generation of white precipitate in the white fungus powdered sample solution of stove drying, qualification result is that residual quantity is greater than 1 μ g/g containing sulfur dioxide residue in sample.The white fungus powdered sample solution of natural drying is then clarified very much, and qualification result there is not sulfur dioxide residue in sample.Come to the same thing with the present embodiment after adopting other method validation beyond the present invention.
Embodiment 3:
Accurately take the Radix Astragali fine powder of 10g stove drying drying and natural drying, add in two round-bottomed flasks respectively, then adopt following same method to identify the sulfur content in two kinds of Chinese crude drugs.Add 150mL distilled water, ultrasound wave process 10 minutes.Then in bottle, 1:1 hydrochloric acid solution 50mL is added.Round-bottomed flask is connected distilling apparatus, adds thermal distillation, cut 0.2mol/L sodium hydroxide solution is collected.After distillation terminates, regulate cut solution ph to 8.0.In solution, add hydrogen peroxide (30%) and heat.Solution is concentrated into 10mL, and it is in the 5ml calcium nitrate solution of 1mmol/L that gained solution drops to concentration.Observe the generation of white precipitate in the Milkvetch Root sample solution of stove drying, qualification result is that residual quantity is greater than 1 μ g/g containing sulfur dioxide residue in sample.The Milkvetch Root sample solution of natural drying is then clarified very much, and qualification result there is not sulfur dioxide residue in sample.Come to the same thing with the present embodiment after adopting other method validation beyond the present invention.
Embodiment 4:
Accurately take the Radix Codonopsis fine powder of 5g stove drying drying and natural drying, add in two round-bottomed flasks respectively, then adopt following same method to identify the sulfur content in two kinds of Chinese crude drugs.Add 150mL distilled water, ultrasound wave process 10 minutes.Then in bottle, 1:1 hydrochloric acid solution 50mL is added.Round-bottomed flask is connected distilling apparatus, adds thermal distillation, cut 0.1mol/L sodium hydroxide solution is collected.After distillation terminates, regulate cut solution ph to 6.0.In solution, add hydrogen peroxide (30%) and heat.Solution is concentrated into 10mL, and it is in the 5ml barium nitrate solution of 1mmol/L that gained solution drops to concentration.Observe the generation of white precipitate in the Radix Codonopsis powder sample solution of stove drying, qualification result is that residual quantity is greater than 1 μ g/g containing sulfur dioxide residue in sample.The Radix Codonopsis powder sample solution of natural drying is then clarified very much, and qualification result there is not sulfur dioxide residue in sample.Come to the same thing with the present embodiment after adopting other method validation beyond the present invention.
Claims (8)
1. the authentication method that Chinese crude drug sulphur is residual, is characterized in that comprising the following steps:
Step one desampling: get Chinese crude drug, is ground into fine powder; Accurately take Chinese crude drug fine powder 2 ~ 10g and put into flask, add distilled water, ultrasound wave process 5 ~ 15 minutes; Then in bottle, hydrochloric acid solution is added; Flask is connected on distilling apparatus, adds thermal distillation, absorb cut with strong base solution; After distillation terminates, regulate cut solution ph to 6.0 ~ 8.0, obtain solution a;
Step 2 sample oxidation: add oxygenant in solution a, adds thermal response 8 ~ 12 minutes, then concentrates, obtain solution b;
Step 3 sample identification: be added dropwise to certain volume solution b in precipitant solution, generates if observe precipitation, then contain sulfur dioxide residue in sample, and residual quantity is more than or equal to 1 μ g/g; Otherwise then in sample, sulfur dioxide residual quantity is less than 1 μ g/g.
2. the authentication method that Chinese crude drug sulphur according to claim 1 is residual, is characterized in that: the granularity of fine powder described in step one is less than 1mm.
3. the authentication method that Chinese crude drug sulphur according to claim 1 is residual, it is characterized in that: in step one, the volume of distilled water is 150mL, vapo(u)rizing temperature is 90 ~ 110 DEG C, and ultrasonic treatment time is 10 minutes, and the volumetric concentration of used salt acid solution is 1:1, the consumption of hydrochloric acid solution is 50mL, strong base solution is sodium hydroxide solution or potassium hydroxide solution, and strong base solution concentration is 0.05 ~ 0.2mol/L, and the cut liquor capacity distilled out is 50 ~ 70mL.
4. the authentication method that Chinese crude drug sulphur according to claim 3 is residual, is characterized in that: oxygenant described in step 2 is hydrogen peroxide or ozone, and the heating reaction time is 10 minutes, and the solution b volume after concentrated in step 2 is 10mL.
5. the authentication method that Chinese crude drug sulphur according to claim 4 is residual, is characterized in that: precipitation agent described in step 3 is water miscible calcium salt, lead salt or barium salt; The concentration of precipitant solution is 0.1 ~ 10mmol/L, and the consumption of precipitant solution is not more than 10mL.
6. the authentication method that Chinese crude drug sulphur according to claim 5 is residual, is characterized in that: precipitation agent is any one in calcium nitrate, plumbi nitras, barium nitrate, lime chloride or barium chloride.
7. the authentication method that Chinese crude drug sulphur according to claim 5 is residual, is characterized in that: the Chinese crude drug fine powder amount in step one is 5g; Vapo(u)rizing temperature is 100 DEG C; Strong base solution is concentration is 0.1mol/L sodium hydroxide solution or potassium hydroxide solution; The liquid volume distilled out is 60mL; Oxygenant described in step 2 is hydrogen peroxide; Precipitation agent described in step 3 is barium chloride.
8. the authentication method that the Chinese crude drug sulphur according to claim 1 ~ 7 any one is residual, is characterized in that: described Chinese crude drug is one or more the combination in ginseng, Radix Codonopsis, American Ginseng, the root of Dahurain angelica, Chinese yam, lily, matrimony vine, the Radix Astragali, chrysanthemum, honeysuckle, white fungus.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105866325A (en) * | 2016-04-28 | 2016-08-17 | 苏州市天灵中药饮片有限公司 | Detection method for residual amount of sulfur dioxide in traditional Chinese medicine decoction pieces |
| CN110790618A (en) * | 2019-11-01 | 2020-02-14 | 南京理工大学 | Method for removing residual sulfur on surface of propellant powder |
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| CN103969261A (en) * | 2014-05-12 | 2014-08-06 | 内蒙古工业大学 | Method for measuring sulfur content of steppe plant |
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| CN103969261A (en) * | 2014-05-12 | 2014-08-06 | 内蒙古工业大学 | Method for measuring sulfur content of steppe plant |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105866325A (en) * | 2016-04-28 | 2016-08-17 | 苏州市天灵中药饮片有限公司 | Detection method for residual amount of sulfur dioxide in traditional Chinese medicine decoction pieces |
| CN110790618A (en) * | 2019-11-01 | 2020-02-14 | 南京理工大学 | Method for removing residual sulfur on surface of propellant powder |
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