CN106248861B - A kind of detection method of pangolin scale Quality Identification - Google Patents
A kind of detection method of pangolin scale Quality Identification Download PDFInfo
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Abstract
The invention discloses a kind of detection method for being capable of Rapid identification pangolin scale quality, this method includes：1）Product to be detected is ground and dissolved with organic solvent；2）It is molten with water weight after the organic solvent of drying dissolving, and carry out low-temperature treatment；3）Sample is analyzed with the chromatography of ions.This method is simple and convenient, and accuracy is high, and effect is preferable, and the defects of conventional detection means can be overcome.
Description
Technical field
The present invention relates to a kind of traditional Chinese medicine quality identification detection method, more particularly to a kind of pangolin scale Quality Identification
Detection method and application, belong to Pharmaceutical Analysis technology and Drug's control field.
Background technology
Pangolin derives from Manidae animal pangolin Manis pentadactyla Linnaeus scale and shell, has and lives
Xue Xiao Disorder, stimulate the menstrual flow lower breast, detumescence and apocenosis, the effect of searching wind and removing obstruction in channels, for Jing Bi Disorder lumps in the abdomen, alactation, carbuncle sore tumefacting virus, rheumatism numbness
Bitterly, the diseases such as paralysis due to windstroke, numbness contracture.Clinically typically use its processed product：Stir-baked SQUAMA MANITIS and vinegar naze.Stir-baked SQUAMA MANITIS is to wear mountain
First health product obtains through sand is ironed；Vinegar naze be through sand scald vinegar quench it is obtained.
Pangolin is the wild protection animal of national two level, and its is curative for effect, but raising difficulty is bigger, and medicine resource is tight
Lack, price of medicinal material goes up year by year.To seek exorbitant profit, some illegal retailers of in the market mix chemical addition agent in concocting process and entered
The illegal weightening of row.2013, national Shi Yao general bureaus carried out medicine " two-combats two is built " special campaigns, in Chinese medicine and medicine materical crude slice field
Each province examines to be shown with the report of quality condition Macro or mass analysis, and pangolin piece disqualification rate is 81%, and subject matter is to process
Illegal weightening in journey.By market survey, it is found that the means of the illegal weightening of current pangolin mainly add inorganic salts.
For ensure the public it is safe and effective for medication, safeguard pangolin medicinal material market it is fair and just and protection consumer's interests,
Need to establish the detection method of pangolin scale quality, strengthen the quality control of the kind, hit pangolin for supervision department and disobey
Method weightening provides technical support.In the research data of pangolin quality standard and its correlation, sample is controlled with total ash inspection
The purity of product, but the method specificity is not strong, and sensitivity is not high；And on the other hand, the mode of conventional chromatography of ions is difficult detection
To the pangolin scale that processing is eluted after weightening.Therefore, it is necessary to which find a kind of new method carries out matter to pangolin scale
Amount detection.
The content of the invention
It is an object of the invention to provide a kind of detection method for pangolin scale Quality Identification.
The present invention is achieved through the following technical solutions above-mentioned purpose：
The quantitative detecting method of inorganic salts is illegally added in a kind of pangolin, is comprised the following steps：
(1) product to be detected is ground and dissolved with organic solvent；
(2) it is molten with water weight after the organic solvent of drying dissolving, and carry out low-temperature treatment；
(3) sample is analyzed with the chromatography of ions.
Preferably, organic solvent is ethyl acetate.
It is further preferred that it is 0~60 DEG C with organic solvent solution temperature.
Preferably, freezing processing temperature is -10~-25 DEG C.
It is further preferred that the freezing processing time is 2~5h.
Preferably, chromatography of ions condition is：
1) anion chromatographic：Chromatographic column is anion-exchange column IonPac AS11-HC (4 × 250mm), leacheate
Concentration is 0~30min 10mmol/L potassium hydroxide solution, and electric conductivity detector, flow velocity 1.0mL/min, detection mode is the moon
Ion Suppressor conductivity detection, sample size are 25 μ L；
2) cation chromatography：Chromatographic column is cation-exchange chromatography post IonPac CS12A (4 × 250mm), and leacheate is dense
Spend and press down for 0~20min 5mmol/L sulfuric acid solution, electric conductivity detector, flow velocity 1.0mL/min, detection mode for cation
Conductivity detection processed, sample size are 25 μ L.
A kind of detection method of pangolin scale, it comprises the following steps：
1) testing sample is ground, and adds 55~60 DEG C of ethyl acetate and fully vibrate；
2) ethyl acetate in above-mentioned steps is dried, adds water fully to be dissolved, -15~-25 DEG C low is used after dissolving
Warm 2~4h of freezing processing；
3) plus after water thawing fully shake up, draw liquid to be detected and sample is analyzed using the method for chromatography of ions,
Chromatogram correlated condition is：
Anion chromatographic：Chromatographic column is anion-exchange column IonPac AS11-HC (4 × 250mm), and leacheate is dense
Spend for 0~30min 10mmol/L potassium hydroxide solution, electric conductivity detector, flow velocity 1.0mL/min, detection mode for it is cloudy from
Sub- Suppressor conductivity detection, sample size are 25 μ L；
Cation chromatography：Chromatographic column is cation-exchange chromatography post IonPac CS12A (4 × 250mm), eluent concentration
Suppress for 0~20min 5mmol/L sulfuric acid solution, electric conductivity detector, flow velocity 1.0mL/min, detection mode for cation
Conductivity detection, sample size are 25 μ L.
The beneficial effects of the invention are as follows：The foundation of the inventive method, it can quickly and efficiently judge whether pangolin medicine materical crude slice is deposited
In illegal weightening behavior, public's drug safety and consumer's interests have been ensured.
Brief description of the drawings
Fig. 1 is SO in anion chromatographic4 2-And Cl-Reference substance chromatography of ions figure.
Fig. 2 is the chromatography of ions figure of pangolin positive in anion chromatographic.
Fig. 3 is the chromatography of ions figure of pangolin negative sample in anion chromatographic.
Fig. 4 is Mg in cation chromatography2+、Na+、K+Reference substance chromatography of ions figure.
Fig. 5 is the chromatography of ions figure of pangolin positive in cation chromatography.
Fig. 6 is the chromatography of ions figure of pangolin negative sample in cation chromatography.
Fig. 7 is the chromatography of ions figure of pure water.
Embodiment
Technical scheme is further illustrated below by way of specific embodiment, but not as to the present invention program's
Limit.
The quality testing of comparative example pangolin scale
The preparation of 1.1 ion concentration standard curves：Precision measures single element standard liquid (1000 μ g/mL) respectively, adds water
Be made every 1mL respectively containing μ g of salt ion 0.1,1 μ g, 5 μ g, 10 μ g, 50 μ g, 100 μ g serial mixed standard solution, carry out color
Spectrum, the standard curve of chromatography of ions is prepared according to the peak area of correlation.
1.2 chromatographic condition：
A. anion chromatographic：Chromatographic column is anion-exchange column IonPac AS11-HC (4 × 250mm), leacheate
Concentration is 0~30min 10mmol/L potassium hydroxide solution, and electric conductivity detector, flow velocity 1.0mL/min, detection mode is the moon
Ion Suppressor conductivity detection, sample size are 25 μ L.
B. cation chromatography：Chromatographic column is cation-exchange chromatography post IonPac CS12A (4 × 250mm), and leacheate is dense
Spend and press down for 0~20min 5mmol/L sulfuric acid solution, electric conductivity detector, flow velocity 1.0mL/min, detection mode for cation
Conductivity detection processed, sample size are 25 μ L.
1.3 quality testing：By pangolin standard items and pass through NaCl, MgSO4, KCl weightenings processing after pangolin it is to be measured
Product are smashed to pieces to powdered, weigh pangolin powder 1.5g, molten with 25mL water weight, are fully vibrated 30min, are added water to be settled to 100mL,
Shake up filtering and carry out chromatography of ions.
The quality testing (1) of the pangolin scale of embodiment 1
By pangolin standard items and pass through NaCl, MgSO4, KCl weightenings processing after pangolin product to be tested smash to pieces to powder
Shape, weigh pangolin powder 1.5g, first with 50mL ethyl acetate 60 DEG C dissolved, fully mix stirring after dry, use 25mL
Water weight is molten, fully vibrates 30min, -20 DEG C of freezing processing 4h.Add water to be settled to 100mL, shake up filtering and carry out chromatography of ions.Color
Spectral condition is according to described in comparative example.
The quality testing (2) of the pangolin scale of embodiment 2
By pangolin standard items and pass through NaCl, MgSO4, KCl weightenings processing after pangolin product to be tested smash to pieces to powder
Shape, pangolin powder 1.5g is weighed, it is molten with 25mL water weight, fully vibrate 30min, -15 DEG C of freezing processing 4h.Water is added to be settled to
100mL, shake up filtering and carry out chromatography of ions.Chromatographic condition is according to described in comparative example.
The quality testing (3) of the pangolin scale of embodiment 3
By pangolin standard items and pass through NaCl, MgSO4, KCl weightenings processing after pangolin product to be tested smash to pieces to powder
Shape, weigh pangolin powder 1.5g, first with 50mL ethyl acetate 37 DEG C dissolved, fully mix stirring after dry, use 25mL
Water weight is molten, fully vibrates 30min, -15 DEG C of freezing processing 4h.Add water to be settled to 100mL, shake up filtering and carry out chromatography of ions.Color
Spectral condition is according to described in comparative example.
The quality testing (4) of the pangolin scale of embodiment 4
By pangolin standard items and pass through NaCl, MgSO4, KCl weightenings processing after pangolin product to be tested smash to pieces to powder
Shape, weigh pangolin powder 1.5g, first with 50mL ethyl acetate 55 DEG C dissolved, fully mix stirring after dry, use 25mL
Water weight is molten, fully vibrates 30min, -25 DEG C of freezing processing 2h.Add water to be settled to 100mL, shake up filtering and carry out chromatography of ions.Color
Spectral condition is according to described in comparative example.
The quality testing (5) of the pangolin scale of embodiment 5
By pangolin standard items and pass through NaCl, MgSO4, KCl weightenings processing after pangolin product to be tested smash to pieces to powder
Shape, weigh pangolin powder 1.5g, first with 50mL ethyl acetate 55 DEG C dissolved, fully mix stirring after dry, use 25mL
Water weight is molten, fully vibrates 30min, -15 DEG C of freezing processing 3h.Add water to be settled to 100mL, shake up filtering and carry out chromatography of ions.Color
Spectral condition is according to described in comparative example.
The quality testing (6) of the pangolin scale of embodiment 6
By pangolin standard items and pass through NaCl, MgSO4, KCl weightenings processing after pangolin product to be tested smash to pieces to powder
Shape, weigh pangolin powder 1.5g, first with 50mL ethyl acetate 0 DEG C dissolved, fully mix stirring after dry, with 25mL water
Weight is molten, fully vibrates 30min, and -10 DEG C of freezing processings handle 5h.Add water to be settled to 100mL, shake up filtering and carry out chromatography of ions.
Chromatographic condition is according to described in comparative example.
The experimental data contrast of 7 each processing method of embodiment
According to comparative example and the processing method of embodiment 1~6, pangolin scale is detected, according to testing result,
Salt ion content in sample is calculated according to the standard curve of comparative example 1.1.Its result is following, and (content unit mg/g, i.e., every gram is worn
Milligram number containing salt ion in naze scale)：
The content of the anion of table 1
The content of the cation of table 2
The as shown by data of above table, take conventional chromatography of ions detection method, can not detect well by
Salt ion content in the illegal weightening pangolin scale of specially treated, and it is non-to use the technical program detection equally to handle
The pangolin scale of method weightening, the data of higher salt ion content can be substantially detected, therefore the technical program can carry
The recall rate for the pangolin scale that height illegally increases weight, avoids the shortcomings that conventional detection means false negative is too high.
Above example is only to introduce the preferred case of the present invention, to those skilled in the art, without departing substantially from this
Any obvious changes and improvements carried out in the range of spirit, it is regarded as the part of the present invention.
Claims (6)
1. illegally adding the quantitative detecting method of inorganic salts in a kind of pangolin, it comprises the following steps：
1) detected sample is ground and dissolved with organic solvent；The organic solvent is ethyl acetate；
2) it is molten with water weight after the organic solvent of drying dissolving, and freezing processing is carried out, add constant volume after water thawing；
3) sample is analyzed with chromatography of ions.
2. detection method according to claim 1, it is characterised in that：The temperature dissolved with organic solvent is 0~60
℃。
3. detection method according to claim 1, it is characterised in that：Freezing processing temperature is -10~-25 DEG C.
4. detection method according to claim 1, it is characterised in that：The freezing processing time is 2~5h.
5. detection method according to claim 1, its chromatographic condition are：
1) anion chromatographic：Chromatographic column is anion-exchange column IonPac AS11-HC, 4 × 250mm of specification, and leacheate is dense
Spend for 0~30min 10mmol/L potassium hydroxide solution, electric conductivity detector, flow velocity 1.0mL/min, detection mode for it is cloudy from
Sub- Suppressor conductivity detection, sample size are 25 μ L；
2) cation chromatography：Chromatographic column is cation-exchange chromatography post IonPac CS12A, 4 × 250mm of specification, eluent concentration
Suppress for 0~20min 5mmol/L sulfuric acid solution, electric conductivity detector, flow velocity 1.0mL/min, detection mode for cation
Conductivity detection, sample size are 25 μ L.
6. illegally adding the quantitative detecting method of inorganic salts in a kind of pangolin, it comprises the following steps：
1) after testing sample is ground, 55~60 DEG C of ethyl acetate is added and are fully vibrated；
2) ethyl acetate in above-mentioned steps is dried, adds water fully to be dissolved, -15~-25 DEG C of low temperature cold is used after dissolving
Freeze 2~4h of processing；
3) plus after water thawing fully shake up, draw liquid to be detected and sample is analyzed using the method for chromatography of ions, chromatogram
Correlated condition is：
Anion chromatographic：Chromatographic column is anion-exchange column IonPac AS11-HC, 4 × 250mm of specification, eluent concentration
It is anion for 0~30min 10mmol/L potassium hydroxide solution, electric conductivity detector, flow velocity 1.0mL/min, detection mode
Suppressor conductivity detection, sample size are 25 μ L；
Cation chromatography：Chromatographic column is cation-exchange chromatography post IonPac CS12A, 4 × 250mm of specification, and eluent concentration is
0~20min 5mmol/L sulfuric acid solution, electric conductivity detector, flow velocity 1.0mL/min, detection mode are that cation suppresses electricity
Detection is led, sample size is 25 μ L.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB9325144D0 (en) * | 1993-12-08 | 1994-02-09 | Medhurst Adam C | Pangolin cricket armour |
| CN105044248A (en) * | 2015-06-04 | 2015-11-11 | 丽珠集团利民制药厂 | Quantitative detection method of edetate disodium and sodium pyrosulfite in Shenqifuzheng injection |
-
2016
- 2016-08-22 CN CN201610702096.5A patent/CN106248861B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB9325144D0 (en) * | 1993-12-08 | 1994-02-09 | Medhurst Adam C | Pangolin cricket armour |
| CN105044248A (en) * | 2015-06-04 | 2015-11-11 | 丽珠集团利民制药厂 | Quantitative detection method of edetate disodium and sodium pyrosulfite in Shenqifuzheng injection |
Non-Patent Citations (4)
| Title |
|---|
| 四种穿山甲属动物类药材的生药鉴别研究;吴芝园;《中国优秀硕士学位论文全文数据库 医药卫生科技辑》;20160215(第02期);E057-7 * |
| 炮山甲二氧化硫残留量超标原因分析与探讨;赵锦燕;《中国优秀硕士学位论文全文数据库 医药卫生科技辑》;20160315(第03期);第16页第1.1-1.4节 * |
| 离子色谱-抑制电导法分别测定海水中阴离子和阳离子;郭莹莹等;《理化检验-化学分册》;20060318;第42卷(第3期);第185～188页 * |
| 离子色谱法测定土壤中无机阴阳离子含量;杨春霞等;《理化检验-化学分册》;20121018;第48卷(第10期);第1199～1202页 * |
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