CN108918517A - A method of the magnesium sulfate illegally added in detection Chinese medicine and medicine materical crude slice - Google Patents
A method of the magnesium sulfate illegally added in detection Chinese medicine and medicine materical crude slice Download PDFInfo
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- CN108918517A CN108918517A CN201810459690.5A CN201810459690A CN108918517A CN 108918517 A CN108918517 A CN 108918517A CN 201810459690 A CN201810459690 A CN 201810459690A CN 108918517 A CN108918517 A CN 108918517A
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- precipitating
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/82—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a precipitate or turbidity
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
Abstract
The invention discloses a kind of methods that detection Chinese medicine and medicine materical crude slice illegally add magnesium sulfate, combine the sulfate radical reaction and magnesium ion reaction of high specificity, screening is carried out for the magnesium sulfate in Chinese medicine, operation of the present invention is easy, quick, high sensitivity, false positive is low and requires detection device low, personnel are supervised for base's medicine and each production and operation enterprise carries out the high-volume screening of Chinese medicine and medicine materical crude slice, efficiently control Chinese medicine and prepared slice quality.
Description
Technical field
The invention belongs to traditional Chinese medicine ingredients detection fields, and in particular to a kind of detection Chinese medicine and medicine materical crude slice illegally add magnesium sulfate
Method.
Background technique
In recent years, with the generally rise of Chinese medicine price, nothing is illegally mixed on the Chinese medicines such as umbellate pore furgus, rhizoma atractylodis, the stem pith of the rice-paper plant
Machine salt magnesium sulfate, to increase weight, to improve selling price.Magnesium salts is white powder, because being easy to get and occupying certain weight
Amount, often penetrates into drug by illegal retailer.In order to effectively hit this kind of fake and inferior Chinese medicines, it is necessary to establish a kind of quick, quasi-
Really, effectively to the rapid screening method of inspection of the incorporation fake and inferior Chinese medicine of magnesium sulfate, reach to control and make and sell disobeying for fake and inferior Chinese medicine
The effect of judicial act.
Summary of the invention
It is an object of the present invention to provide a kind of methods for the magnesium sulfate that detection Chinese medicine and medicine materical crude slice illegally add.
Still a further object of the present invention is to provide a kind of detection Chinese medicine and medicine materical crude slice illegally adds the kit of magnesium sulfate.
The technical solution adopted by the present invention is that：
A kind of kit detecting the magnesium sulfate illegally added in Chinese medicine and medicine materical crude slice, contains detection sulfate ion and magnesium
The reagent of ion.
Further, the reagent includes acetic acid lead solution, sodium hydroxide solution and iodine solution.
A method of the magnesium sulfate illegally added in detection Chinese medicine and medicine materical crude slice, steps are as follows：
(1) Chinese medicine and/or medicine materical crude slice are added to the water, solid-liquid ratio 1g：5~10mL stands after stirring and supernatant is taken to obtain
Sample prepare liquid；
(2) it takes a part of sample prepare liquid that lead acetate test solution is added dropwise, sees whether to generate white precipitate；If it is heavy to generate white
It forms sediment, sodium hydroxide is added dropwise into precipitating, whether there is or not reduction or dissolutions for observation precipitating；If white precipitate reduces or dissolution, illustrate sample
Product contain sulfate ion；
(3) it takes another part sample prepare liquid that sodium hydroxide is added dropwise, sees whether to generate white precipitate；If it is heavy to generate white
It forms sediment, precipitating is divided into two parts, excessive sodium hydroxide is added dropwise in portion precipitating, and whether there is or not be completely dissolved for observation precipitating；Another precipitating
Iodine solution is added dropwise, whether observation precipitating becomes rufous；If it is insoluble that white precipitate after excessive sodium hydrate is added dropwise, and white precipitate
Become rufous after adding iodine solution, then illustrates to contain magnesium ion in sample.
Further, in step (1), Chinese medicine and/or medicine materical crude slice are added water and first shred before.
Further, mixing time described in step (1) is 2~15min.
Further, time of repose described in step (1) is 15~20min.
Further, the Chinese medicine and medicine materical crude slice include pig Fu, Poria cocos, fuling peel, rhizoma zingiberis, campanulaceae, arisaema cum bile, Radix Glycyrrhizae,
Blackberry lily, Radix Codonopsis, safflower, Cortex Phellodendri, rhizoma atractylodis, cortex dictamni, rheum officinale, the coptis, Radix Salviae Miltiorrhizae, Chinese yam, the root of straight ladybell, radix aucklandiae, cordyceps sinensis, ginseng, bird's nest,
Pangolin.
The beneficial effects of the invention are as follows：
For the magnesium sulfate illegally added in Chinese medicine and medicine materical crude slice, sulfate radical reaction and the magnesium ion of high specificity are combined
Reaction carries out screening, and operation of the present invention simplicity, quick, high sensitivity, false positive is low, and of less demanding to detection device, for
Base's medicine supervises personnel and each production and operation enterprise carries out the high-volume screening of Chinese medicine and medicine materical crude slice, for improving Chinese medicine and medicine materical crude slice
Quality is of great significance.
Detailed description of the invention
Fig. 1 is umbellate pore furgus feminine gender, the supernatant prepare liquid of positive sample and contrast agent (2% magnesium sulfate).
Fig. 2 is that sodium hydroxide is added dropwise in negative umbellate pore furgus, positive sample and contrast agent (2% magnesium sulfate) to generate precipitating.
Fig. 3 is that negative umbellate pore furgus, positive sample and contrast agent (2% magnesium sulfate) generation precipitating are further continued for that excessive hydrogen-oxygen is added dropwise
It is insoluble to change sodium precipitating.
Fig. 4 is that umbellate pore furgus negative, positive sample and contrast agent (2% magnesium sulfate) generate precipitating iodine test solution are added dropwise again and redden palm fibre
Color.
Fig. 5 is umbellate pore furgus feminine gender, the supernatant prepare liquid of positive sample and contrast agent (2% magnesium sulfate).
Fig. 6 is that negative umbellate pore furgus, positive sample and the middle dropwise addition lead acetate test solution generation white of contrast agent (2% magnesium sulfate) are heavy
It forms sediment.
Fig. 7 is that negative umbellate pore furgus, positive sample and contrast agent (2% magnesium sulfate) dropwise addition lead acetate test solution are further continued for being added dropwise
Sodium hydroxide pellets are measured to reduce or dissolve.
Fig. 8 is the Adlerika figure of 0.05%, 0.1%, 0.5%, 1%, 2%, 4%, 6% 7 various concentration.
Fig. 9 is that the three drop sodium hydroxides of Adlerika dropwise addition of seven various concentrations precipitate.
Figure 10 is added dropwise acetic acid lead solution for the Adlerika generation precipitating of seven various concentrations again and precipitates.
Figure 11 is after acetic acid lead solution is added dropwise in the Adlerika of seven various concentrations to be further continued for that sodium hydroxide pellets are added dropwise
It reduces.
Specific embodiment
The present invention is further illustrated with reference to the accompanying drawing, but is not limited to embodiment.
Embodiment 1
Material：Pig Fu, Poria cocos, fuling peel, rhizoma zingiberis, campanulaceae, arisaema cum bile, Radix Glycyrrhizae, blackberry lily, Radix Codonopsis, safflower, Cortex Phellodendri, rhizoma atractylodis,
Cortex dictamni, rheum officinale, the coptis, Radix Salviae Miltiorrhizae, Chinese yam, the root of straight ladybell, radix aucklandiae, cordyceps sinensis, ginseng, bird's nest, the sample of kind 510 of pangolin 23 are equal
From being purchased from pharmacy and market.
Method：(1) Chinese medicine：Sample about 4g uniformly is weighed, shreds and is put into beaker, add distilled water about 20ml, make
Including sample is totally submerged, stirring stood 15 minutes after 2 minutes, took supernatant as sample solution to be measured；
Traditional Chinese medicinal herbs from entire grass：It takes 20g sample to shred mixing, therefrom extracts about 4g and be put into beaker, add distilled water about 50ml,
Including being totally submerged sample, stirring stood 15 minutes after 2 minutes, took supernatant as sample solution to be measured.
(2) magnesium ion reacts：It takes 2ml sample solution to be measured to be placed in test tube (Fig. 1), sodium hydroxide test solution 3~5 is added dropwise
Drop sees whether to generate white precipitate (Fig. 2)；If there is precipitating to generate, supernatant is abandoned, precipitating is divided into two parts and is placed in new test tube
In：Wherein continue to be added dropwise sodium hydroxide test solution to excess for 1 part, whether observation precipitating is completely dissolved (Fig. 3)；Another 1 part of dropwise addition iodine examination
Liquid 3~5 drips, and whether observation precipitating from white becomes rufous (Fig. 4).
(3) sulfate radical reacts：It takes 2ml sample solution to be measured to be placed in test tube (Fig. 5), lead acetate test solution 3~5 is added dropwise and drips,
It sees whether to generate white precipitate (Fig. 6)；If there is precipitating to generate, then the drop of sodium hydroxide test solution 20 is added dropwise, whether observation precipitating subtracts
Less or dissolve (Fig. 7).
Embodiment 2
Method：(1) Chinese medicine：Sample about 4g uniformly is weighed, shreds and is put into beaker, add distilled water about 30ml, make
Including sample is totally submerged, stirring stands 10 minutes after ten minutes, takes supernatant as sample solution to be measured；
Traditional Chinese medicinal herbs from entire grass：It takes 20g sample to shred mixing, therefrom extracts about 5g and be put into beaker, add distilled water about 50ml,
Including being totally submerged sample, stirring stands 10 minutes after ten minutes, takes supernatant as sample solution to be measured.
(2) magnesium ion reacts：It takes 2ml sample solution to be measured to be placed in test tube, sodium hydroxide test solution 3~5 is added dropwise and drips, observation
Whether white precipitate is generated；If there is precipitating to generate, supernatant is abandoned, precipitating is divided into two parts and is placed in new test tube：Wherein 1 part after
To excess, whether observation precipitating is completely dissolved the continuous sodium hydroxide test solution that is added dropwise；Another 1 part of dropwise addition iodine test solution 3~5 drop, observation precipitating
Whether from white rufous is become.
(3) sulfate radical reacts：It takes 2ml sample solution to be measured to be placed in test tube, lead acetate test solution 3~5 is added dropwise and drips, observation is
No generation white precipitate；If there is precipitating to generate, then the drop of sodium hydroxide test solution 20 is added dropwise, whether observation precipitating reduces or dissolve.
Embodiment 3
Method：(1) Chinese medicine：Sample about 4.5g uniformly is weighed, shreds and is put into beaker, add distilled water about 45ml,
Including being totally submerged sample, stirring stood 20 minutes after 15 minutes, took supernatant as sample solution to be measured；
Traditional Chinese medicinal herbs from entire grass：It takes 20g sample to shred mixing, therefrom extracts about 5g and be put into beaker, add distilled water about 50ml,
Including being totally submerged sample, stirring stood 20 minutes after 15 minutes, took supernatant as sample solution to be measured.
(2) magnesium ion reacts：It takes 2ml sample solution to be measured to be placed in test tube, sodium hydroxide test solution 3~5 is added dropwise and drips, observation
Whether white precipitate is generated；If there is precipitating to generate, supernatant is abandoned, precipitating is divided into two parts and is placed in new test tube：Wherein 1 part after
To excess, whether observation precipitating is completely dissolved the continuous sodium hydroxide test solution that is added dropwise；Another 1 part of dropwise addition iodine test solution 3~5 drop, observation precipitating
Whether from white rufous is become.
(3) sulfate radical reacts：It takes 2ml sample solution to be measured to be placed in test tube, lead acetate test solution 3~5 is added dropwise and drips, observation is
No generation white precipitate；If there is precipitating to generate, then the drop of sodium hydroxide test solution 20 is added dropwise, whether observation precipitating reduces or dissolve.
As a result：The selection result is shown in Table 1, table 2 and table 3 (data are as follows), and test result shows 10 batches of umbellate pore furgus, 7 batches of rhizoma atractylodis inspections
Contain sulfuric acid magnesium component out.
Magnesium sulfate in 1 umbellate pore furgus of watch sieves result fastly
Conclusion：The sample survey of number 8,11,12,13,15,16,17,19,20,25 contain as the result is shown magnesium sulfate at
Point.
Magnesium sulfate in 2 rhizoma atractylodis of watch sieves result fastly
Conclusion：The sample survey that number is 3,11,12,19,20,23,25 contains sulfuric acid magnesium component as the result is shown.
3 sample magnesium sulfate of watch sieves result fastly
Note：Sulfate radical reaction, magnesium ion reaction should be positive (+) in positive and negative；Number represents lot number.
4 sample soaking time of embodiment is investigated
Method：Sample 5g uniformly is weighed, shreds, is put into beaker, adds distilled water about 30ml to be totally submerged sample, after stirring
5,10,15 minutes are stood, the supernatant of different periods is taken to be operated according to embodiment 1 respectively.
Traditional Chinese medicinal herbs from entire grass：It takes 20g sample to shred, mixes, take about 5g to be put into beaker, distilled water about 60ml is added to make sample
It is totally submerged, stands 5,10,15 minutes after stirring, take different periods respectively takes supernatant according to embodiment 1 the step of progress
Operation.
As a result：The aobvious chemical reaction of supernatant in different time periods, but find after being stirred sample and standing 15 minutes
Supernatant effect is most obvious.
5 sensitivity test of embodiment
Method：It is appropriate to weigh magnesium sulfate powder, distilled water is added to be configured to solution, sulfuric acid content of magnesium is respectively 0.05%,
0.1%, 0.5%, 1%, 2%, the 4%, solution of 6% 7 kind of various concentration, according to being found after being operated the step of embodiment 1,
0.5%, 1%, 2%, 4% and 6% Adlerika generates apparent chemical reaction.
As a result：Test result shows that 0.5%, 1%, 2%, 4% and 6% Adlerika generates apparent positive reaction,
Reacting phenomenon is obvious (being shown in Table 4).Experimental phenomena is shown in Fig. 8~11：Fig. 8 is 0.05%, 0.1%, 0.5%, 1%, 2%, 4%, 6%
The Adlerika of seven various concentrations, Fig. 9 are that the three drop sodium hydroxides of Adlerika dropwise addition of various concentration precipitate, and are schemed
10 precipitate for the Adlerika dropwise addition acetic acid lead solution of various concentration, and Figure 11 is that the Adlerika of various concentration is added dropwise
It is further continued for that sodium hydroxide discovery precipitating reduction is added dropwise after acetic acid lead solution.In terms of comprehensive, 0.5%, 1%, 2%, 4% and 6%
Adlerika reacting phenomenon is obvious.
The sensitivity test result of 4 Adlerika of table
Note：It is in positive reaction that "+", which represents, and it is not in positive reaction that "-", which represents,.
The verifying of 6 magnesium ion response assays of embodiment
It is in 10 batches of umbellate pore furgus of positive reaction, 7 batches of rhizoma atractylodis Chinese medicines by front sulfate ion and magnesium ion, using GB/
Quantitative analysis of the T5009.90-2003 to magnesium ion in medicinal material, this 17 batches gone out with atomic absorption spectroscopy determination screening
Magnesium ion in positive sample.
As a result：It was found that the magnesium ion content of positive sample is high compared with the magnesium ion of negative sample, there is (number in non-false positive phenomenon
5~table 6 is shown in Table under).
The measurement of 5 umbellate pore furgus positive sample magnesium ion content of table
The measurement of 6 rhizoma atractylodis positive sample magnesium ion content of table
In conclusion this experimental study has collected the Chinese medicine of 23 510 batches of kind altogether, wherein umbellate pore furgus, rhizoma atractylodis this 2
Kind shares the detection of 17 batches and contains sulfuric acid magnesium component.The result shows that adding weight powder " magnesium sulfate ", present invention behaviour for Chinese medicine
Make easy, quick, high specificity, supervises personnel for base's medicine and each production and operation enterprise carries out the high-volume of Chinese medicine and medicine materical crude slice
Screening efficiently controls Chinese medicine and prepared slice quality.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (7)
1. a kind of kit of the magnesium sulfate illegally added in detection Chinese medicine and medicine materical crude slice, which is characterized in that contain detection sulfuric acid
The reagent of radical ion and magnesium ion.
2. kit according to claim 1, which is characterized in that the reagent includes acetic acid lead solution, sodium hydroxide
Solution and iodine solution.
3. a kind of method of the magnesium sulfate illegally added in detection Chinese medicine and medicine materical crude slice, which is characterized in that steps are as follows：
(1) Chinese medicine and/or medicine materical crude slice are added to the water, solid-liquid ratio 1g：5~10mL stands after stirring and supernatant is taken to obtain sample
Prepare liquid；
(2) it takes a part of sample prepare liquid that lead acetate test solution is added dropwise, sees whether to generate white precipitate；If generating white precipitate,
Sodium hydroxide is added dropwise into precipitating, whether there is or not reduce or dissolve for observation precipitating；If white precipitate reduces or dissolution, illustrate that sample contains
There is sulfate ion；
(3) it takes another part sample prepare liquid that sodium hydroxide is added dropwise, sees whether to generate white precipitate；If generating white precipitate,
Precipitating is divided into two parts, excessive sodium hydroxide is added dropwise in portion precipitating, and whether there is or not be completely dissolved for observation precipitating；Another precipitating is added dropwise
Whether iodine solution, observation precipitating become rufous；If it is insoluble that white precipitate after excessive sodium hydrate is added dropwise, and white precipitate adds iodine
Become rufous after liquid, then illustrates to contain magnesium ion in sample.
4. according to the method described in claim 3, it is characterized in that, Chinese medicine and/or medicine materical crude slice are added before water in step (1)
First shred.
5. according to the method described in claim 3, it is characterized in that, mixing time described in step (1) is 2~15min.
6. according to the method described in claim 3, it is characterized in that, time of repose described in step (1) is 15~20min.
7. according to the method described in claim 3, it is characterized in that, the Chinese medicine and medicine materical crude slice include pig Fu, Poria cocos, Poria cocos
Skin, rhizoma zingiberis, campanulaceae, arisaema cum bile, Radix Glycyrrhizae, blackberry lily, Radix Codonopsis, safflower, Cortex Phellodendri, rhizoma atractylodis, cortex dictamni, rheum officinale, the coptis, Radix Salviae Miltiorrhizae, Chinese yam,
The root of straight ladybell, radix aucklandiae, cordyceps sinensis, ginseng, bird's nest, pangolin.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112986230A (en) * | 2021-03-02 | 2021-06-18 | 郑州欧柯奇仪器制造有限公司 | Kit and method for rapidly detecting magnesium sulfate in agaric |
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Application publication date: 20181130 |