CN106596545A - Rapid detection method of sulfonylurea chemical constituents - Google Patents
Rapid detection method of sulfonylurea chemical constituents Download PDFInfo
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- CN106596545A CN106596545A CN201611140069.XA CN201611140069A CN106596545A CN 106596545 A CN106596545 A CN 106596545A CN 201611140069 A CN201611140069 A CN 201611140069A CN 106596545 A CN106596545 A CN 106596545A
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- G—PHYSICS
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- 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
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract
The invention provides a rapid detection method of sulfonylurea chemical constituents. The rapid detection method comprises the following steps: weighing a to-be-detected sample of 1 oral dose, grinding or crushing the sample, adding 2-8mL of a NaOH solution with concentration being 0.001-0.1mol/L, shaking and leaving the solution to stand, filtering a supernatant, adding 0.23-0.30mL of a CuSO4 test solution with concentration being 0.005 mol/L to a filtrate, and determining whether the sample contains sulfonylurea chemical constituents according to the phenomenon of a precipitation reaction. By means of the characteristics that the solubility of NaOH to sulfonylureas and the relative excess NaOH can eliminate interference of an acidic matrix and provide a basic environment for a color reagent, the false positive phenomenon can be prevented, and reaction results can be observed on basis of the precipitation phenomenon. The detection method has the advantages that the adopted reagent is safe, operation is quite simple and convenient, special equipment is not needed, the analysis cost is low, the specificity is high, the sensitivity is high and test results are easy to observe, and is suitable for on-site rapid detection of illegally added sulfonylurea chemical constituents in hypoglycemic Chinese patent drugs and health food.
Description
Technical field
The invention belongs to pharmaceutical technology field, is related to a kind of method of food and medicine analysis, and in particular to a kind of hypoglycemic class
Chinese patent drug and health food illegally add the method for quick of sulfonylureas chemical composition.
Background technology
In recent years, the quantity rapid growth of China diabetic, according to 2010《New England Journal of Medicine》Announce
As a result show, China adult diabetes rate is 9.7%, and early stage illness rate is up to 15.5%.Numerous clinical researches are for sulphur
The efficacy and saferry of carbamide type medicine have accumulated rich experience so as to become current clinically most often applied OHA
One of thing.With active demand of the people to antidiabetic drugs, various drop sugar products are also increasing.Chinese patent drug and health care are eaten
Product are most of to derive from natural materials, is considered to have higher security, is favored by diabetic, but it has action slowly
Or the shortcoming of DeGrain.In order to seek great number interests, part lawless person illegally adds wherein sulfonylureas chemicals
To cheat patient's.
Sulfonylurea drugs are to find earliest and the most widely used oral hypoglycemic drug, due to Chinese patients it is substantially fertile
Person is less based on fat, insulin resistance and price factor of medicine, and this kind of medicine is extremely adapted to China's actual conditions.Sulfonylureas
Medicine has evolved to so far the third generation.First generation sulfonylurea drugs just reach identical hypoglycemic effect because needing oral larger dose
High with the incidence compared with the hypoglycemic reaction caused by second generation sulfonylurea drugs and other bad reactions and present Clinical practice
It is less.At present domestic conventional sulfonylurea drugs have：Glibenclamide, Glimepiride, Glipizide (containing common agent and controlled release agent),
Gliclazide (containing common agent and sustained release tablets) and gliquidone etc..Most of sulfonylurea drugs are equal to be arranged Jing after liver metabolism from kidney
Let out, the only main Jing biliary tracts of gliquidone are discharged, about 5% Jing renal excretions.Sulfonylurea drugs occupy in the treatment of diabetes B
Consequence, but in recent years sulfonylurea drugs cause the side reactions such as hypoglycemia, weightening, cardiovascular event risk gradually to cause
The attention of educational circles.So, if diabetic's long-term taking in the case of unwitting contains sulfonylureas Chinese patent drug and health care
Food, its health can be endangered by different degrees of, and severe patient even can cause death.
For the illegal addition of hypoglycemic medicine in Chinese patent drug and health food, at this stage detection method mainly has following two
Class：
First, instrument detection class
Infra-red sepectrometry, Raman spectroscopy, high performance liquid chromatography and tablets by HPLC-MS can be used to examine
Test in Chinese patent drug and health food and whether illegally add sulfonylureas drugs for diabetes.They all have and quickly, directly detect medicine
Advantage, at the same there is also need to be equipped be inconvenient to carry expensive instrument, have certain requirements limitation to detection environment.
2nd, non-instrument detection
Thin-layered chromatography, chromogenic reaction, the precipitation method can be used to check in Chinese patent drug and health food whether illegally add sulphur
Ureas antidiabetic drug.The advantage of wherein thin-layered chromatography is need not to use large-scale, expensive analytical instrument, it is easy to operate, result it is straight
See and understand, it has the disadvantage to there are certain requirements a plate technique, edge effect, disturbing factor are more.(number of patent application is chromogenic reaction
201310553426.5) analysis cost is low, and specificity is strong, and sensitivity is high, is extracted with dichloromethane, can extract complete.Meanwhile, it is real
Test using dichloromethane and need heating to volatilize and sulfuric acid, respectively poisonous and severe corrosive reagent is bad to human body and environment；
Heating is needed in another step, heating tool need to be equipped with, be not suitable for field quick detection.Heating operation occurs showing for solution ejection
As not safe enough.(number of patent application is for precipitation reaction：200910014666.1), the method sensitivity is high, and specificity is strong, operation
Step is simple, and result of the test substantially, easily observe by phenomenon.Meanwhile, experiment needs to use chloroform, and consumption is big, and needs to be evaporated,
Solvent volatilization is bad to human body and environment in atmosphere.In addition water bath method needs instrument in operating procedure, for fast inspection, carries
Inconvenience.
The content of the invention
In view of the above, it is necessary to which a kind of safety, quick, simple operation, low, the reliable sulphur of environmental condition requirement are provided
The method for quick of ureas chemical composition, to ensure the drug safety of the people.
To solve above-mentioned technical problem, the present invention is adopted the technical scheme that, a kind of quick inspection of sulfonylureas chemical composition
Survey method, comprises the following steps：
1) Chinese patent drug to be measured or appropriate health products are taken, it is finely ground as test sample equivalent to 1 oral dose, it is put into tool plug examination
2-8mL 0.001-0.1mol/L NaOH solutions are added in pipe, 1-5min is shaken, is stood, supernatant liquid filtering, collect filtrate conduct
Test liquid A；
2) 0.23-0.30mL 0.005mol/L CuSO are added dropwise in test liquid A4Observation phenomenon in test solution, 1min；If going out
Now obvious muddy, deposited phenomenon white or azury, can determine whether to contain sulfonylureas chemical composition in test sample.
Above-mentioned steps 1) in, the concentration of NaOH solution is preferably 0.01mol/L can reach optimal reaction effect.
Above-mentioned steps 2) in, CuSO is added dropwise in test liquid A4It is not required to be shaken after test solution, its reason exists
Cause precipitation to spread after concussion, affect observing effect.
The Cleaning Principle of this method is as follows：
The conventional sulfonylureas drugs for diabetes chemical constitution of clinic is as shown in table 1, due in the chemical constitution of sulfonylurea drugs
Delocalization of the sulfonyl to the lone pair electrons conspicuousness on nitrogen-atoms.Their pKa value is about 5.0, therefore aobvious acidity, it is solvable
In NaOH solution, acetone, chloroform, ethanol, water or ether are practically insoluble in.
The chemical constitution of the sulfonylureas hypoglycemic agent of table 1
The present invention is realized to its quick detection using the following property of sulfonylureas chemical composition：
1st, sulfonylurea drugs have uride structure, show acidity, dissolve in NaOH solution, and uride structure with glibenclamide
As a example by, NaOH solution generates glibenclamide sodium salt with glibenclamide reaction, and concrete reaction is as follows：
2nd, NaOH and CuSO4Between reaction
1. complete precipitation reaction：CuSO4It is 1 with the ratio of the amount of NaOH materials:2, gained product is blue cotton-shaped heavy
Form sediment, be long placed in rear upper solution colourless.
Correlated response formula：2NaOH+CuSO4=Cu (OH)2↓+Na2SO4
②CuSO4Excessive response：CuSO4It is more than 1 with the ratio of the amount of NaOH materials:2, gained reactant is light blue alkali formula
Copper sulphate.
Correlated response formula：NaOH+CuSO4→Cux(OH)y SO4↓+3Na2SO4
3. NaOH excessive responses：CuSO41 is less than with the ratio of the amount of NaOH materials:2, gained reactant is blue hydroxide
Copper flocculent deposit, the Kocide SD of generation can occur following two response situations：1. CO in Kocide SD flocculent deposit and solution2
Reaction can generate verdigris (basic copper carbonate)；2. it is blue that the Kocide SD for generating continues reaction generation tetrahydroxy conjunction copper acid sodium with NaOH
Color solution, the solution is stable in strong basicity environment, and dilute alkaline soln is long placed in and easily generate black precipitate (cupric oxide).
Correlated response formula：
2NaOH+CuSO4=Cu (OH)2↓+Na2SO4
2NaOH+CO2=Na2CO3+H2O
Cu(OH)2+Na2CO3→Cu2(OH)2CO3↓
Cu(OH)2+2NaOH→Na2[Cu(OH)4]
Na2[Cu(OH)4]=Na2CuO2+2H2O
Na2CuO2=Na2O+CuO
By above-mentioned NaOH and CuSO43 kinds of response situations it is visible, NaOH and CuSO4Different amounts is than the phenomenon that obtains not
Equally, the present invention uses NaOH excessive responses.Selection gist is：
1) NaOH can excessively exclude acidic matrix interference, it is to avoid false positive phenomenon；
2)0.005mol/L CuSO4With the situation of 0.001-0.1mol/L NaOH solutions reaction：1. 0.005mol/ is added
L CuSO4The amount ＜ 0.30mL of test solution, solution is colourless to light blue solution；2. as addition CuSO4Amount >=the 0.30mL of test solution,
Solution gradually produces blue floccule；Therefore 0.10-0.30mL0.005mol/L CuSO should be chosen4With 0.001-0.1mol/L
NaOH solution this reaction condition can avoid both from reacting generation Cu (OH)2The false positive phenomenon of blue flocculent deposit, wherein NaOH
The concentration of solution is preferably 0.01mol/L can reach optimal reaction effect.
NaOH solution and CuSO4The determination of test solution addition ratio and concentration is according to following three points, one, CuSO4Test solution
The determination of concentration：0.005mol/L CuSO4The light blue copper acid sodium that test solution can be generated with 0.001-0.1mol/L NaOH solutions
Solution, and solution colour with NaOH concentration increase and shoal, work as CuSO4During test solution >=0.01mol/L, solution is easily at once
Generate Cu (OH)2Blue flocculent deposit, forms false positive phenomenon, therefore the present invention by CuSO4Test solution concentration is defined as 0.005mol/L
Can prevent false positive phenomenon from producing；Two, CuSO4The determination of test solution addition：When NaOH solution concentration and addition and sight
When the time examined is fixed, 0.005mol/L CuSO are added4The amount ＜ 0.30mL of test solution, solution is colourless to light blue solution, when
Add CuSO4Amount >=the 0.30mL of test solution, solution gradually produces blue floccule；The three, determination of observing time, when past
0.001-0.1mol/L NaOH solutions add 0.30mL 0.005mol/L CuSO4Test solution, in 0-6min, solution be it is light blue, when
Time, solution engendered blue flocculent deposit more than 6min, false positive phenomenon was formed, when the optimal viewing time is 1min.
3、CuSO4Can carry out in the basic conditions being complexed instead with the aminosulfonyl functional group in sulfonylureas chemical composition
Should, as the 0.005mol/L CuSO being added dropwise4The amount of test solution is more than 0.23mL, and solution is in hypersaturated state, there is Precipitation；
As the 0.005mol/L CuSO being added dropwise4The amount of test solution is 0.10-0.23mL, and solution has following two possibility：1) solution is not in
Saturation state, without Precipitation；2) solution will separate out undecomposed state in saturation is just reached, and precipitation reaches with dissolving
To dynamic equilibrium, not only generate without precipitation but also without precipitation dissolving.
Reaction equation is as follows：
4th, it is above-mentioned visible：
(1), CuSO4In NaOH reactions, as addition CuSO4, there is Cu (OH) in the amount >=0.30mL of test solution2It is blue cotton-shaped
Precipitation.As addition CuSO4The amount ＜ 0.30mL of test solution, solution is colourless to light blue solution.There is Cu after in order to exclude reaction
(OH)2Interference of the blue flocculent deposit to experimental result, therefore add CuSO4The amount ＜ 0.30mL of test solution；
(2) CuSO4In the reaction of sulfonylureas chemical composition, CuSO is added4Amount >=the 0.23mL of test solution, there is Precipitation,
With reference to sulfonylureas chemical composition, CuSO4, NaOH three's response situation, therefore add CuSO4When the amount of test solution is 0.23-0.30mL,
Sulfonylurea drugs are reacted and reach saturation state, it is seen that precipitation；NaOH and CuSO4Test solution reaction reaches insatiable hunger and/or firm saturation
State, without Precipitation.In order to exclude NaOH and CuSO4The false positive precipitation interference that test solution reaction is produced, present invention examination used
The concentration and amount of agent is defined as：0.001-0.1mol/L NaOH solutions and 0.23-0.30mL 0.005mol/L CuSO4Test solution,
The time is after observing response：Observation phenomenon in 1min after reaction.
The present invention compared with prior art, has the beneficial effect that：
1) testing sample only needs the CuSO for extracting, adding low concentration42 steps such as test solution reaction can judge according to precipitation reaction
Whether sample contains sulfonylurea drugs, and extract used, reaction test solution are common chemical reagent, very safe, operation
Simplicity, analysis cost is low.
2) testing sample selects 0.001-0.1mol/L NaOH solutions, exactly using NaOH relatively excessively eliminating acidity
The interference of matrix and sulfonylurea drugs have acid property, with 0.23-0.30mL0.005mol/L CuSO4Test solution is heavy
Shallow lake reactant, is exactly to generate precipitation reaction, this method reaction spirit with aminosulfonyl functional group in the basic conditions using it
Quick, specificity is strong, and phenomenon is obvious, it is not necessary to be equipped with instrument, it is adaptable to field quick detection.
3) present invention is 1mg/ pieces to sulfonylureas sample detection limit, and wherein gliclazide sample detection limit is up to 0.25mg/
Piece.
Specific embodiment
The present invention is further explained with reference to example is embodied as, but is embodied as example and the present invention is not done
Any restriction.
Embodiment 1：Capsule (Jing LC-MS are checked, and this product does not contain sulfonylureas chemical composition)
Testing sample 2 is taken, in putting 10mL tool plug test tubes, 3mL 0.001mol/LNaOH solution is added, 5min is shaken, it is quiet
1min is put, supernatant liquid filtering takes 1mL filtrates and adds 0.25mL 0.005mol/LCuSO4Solution, solution is produced without precipitation.
Interpretation of result：Testing sample solution is produced without precipitation, is shown without sulfonylureas chemical composition in sample, as a result with reality
It is consistent.
Embodiment 2：Capsule (Jing LC-MS are checked, this product chemical composition containing sulfonylureas)
Testing sample 3 is taken, in putting 10mL tool plug test tubes, 8mL 0.01mol/LNaOH solution is added, 2min is shaken, it is quiet
4min is put, supernatant liquid filtering takes 1mL filtrates and adds 0.25mL 0.005mol/LCuSO4Solution, solution has precipitation to produce.
Interpretation of result：Testing sample solution has white precipitate to produce, and shows there is sulfonylureas chemical composition in sample, as a result with
Actually it is consistent.
Embodiment 3：Tablet (Jing LC-MS are checked, and this product does not contain sulfonylureas chemical composition)
2, sample is taken, it is finely ground, in putting 10mL tool plug test tubes, 6mL 0.1mol/LNaOH solution is added, screw, shake
1min stands 2min, and supernatant liquid filtering takes 1mL filtrates and adds 0.25mL0.005mol/LCuSO4Solution, solution is produced without precipitation
It is raw.
Interpretation of result：Testing sample solution is produced without precipitation, is shown without sulfonylureas chemical composition in sample, as a result with reality
It is consistent.
Embodiment 4：Tablet (Jing LC-MS are checked, this product chemical composition containing sulfonylureas)
Testing sample 1 is taken, in putting 10mL tool plug test tubes, 2mL 0.01mol/LNaOH solution is added, 2min is shaken, it is quiet
2min is put, supernatant liquid filtering takes 1mL filtrates and adds 0.25mL 0.005mol/LCuSO4Solution, solution has precipitation to produce.
Interpretation of result：Testing sample solution has white precipitate to produce, and shows there is sulfonylureas chemical composition in sample, as a result with
Actually it is consistent.
Embodiment 5：Granule (Jing LC-MS are checked, this product chemical composition containing sulfonylureas)
Take testing sample 1 to wrap, in putting 10mL tool plug test tubes, add 8mL 0.01mol/LNaOH solution, shake 1min, it is quiet
2min is put, supernatant liquid filtering takes 1mL filtrates and adds 0.25mL 0.005mol/LCuSO4Solution, solution has precipitation to produce.
Interpretation of result：Testing sample solution has white precipitate to produce, and shows there is sulfonylureas chemical composition in sample, as a result with
Actually it is consistent.
Table 1：
| Sample number into spectrum | Formulation | Sampling amount | Reaction result | Identification result | LC-MS assays |
| Sample 1 | Capsule | 2 | Produce without precipitation | It is negative | Without sulfonylureas chemical composition |
| Sample 4 | Capsule | 3 | There is precipitation to produce | It is positive | Chemical composition containing sulfonylureas |
| Sample 3 | Tablet | 2 | Produce without precipitation | It is negative | Without sulfonylureas chemical composition |
| Sample 4 | Tablet | 1 | There is precipitation to produce | It is positive | Chemical composition containing sulfonylureas |
| Sample 5 | Granule | 1 bag | There is precipitation to produce | It is positive | Chemical composition containing sulfonylureas |
Explanation：The commercially available sample medicine of 5 batches is detected using the method for the present invention, and is compared using LC-MS testing results, as a result
As shown in Table 1, the method that the present invention is adopted is identical with LC-MS assays.
Contrast test
Comparative example 1：Capsule (Jing LC-MS are checked, and this product does not contain sulfonylureas chemical composition)
Testing sample 2 is taken, in putting 10mL tool plug test tubes, 3mL 0.01mol/LNaOH solution is added, 2min is shaken, it is quiet
2min is put, supernatant liquid filtering takes 1mL filtrates and adds 0.25mL 0.1mol/LCuSO4Solution, solution has blue precipitate to produce.
Experimental result：Testing sample solution has blue precipitate to produce.
Comparative example 2：Capsule (Jing LC-MS are checked, this product chemical composition containing sulfonylureas)
Testing sample 3 is taken, in putting 10mL tool plug test tubes, 6mL 0.01mol/LNaOH solution is added, 2min is shaken, it is quiet
2min is put, supernatant liquid filtering takes 1mL filtrates and adds 0.25mL 0.05mol/LCuSO4Solution, solution has violet precipitation to produce
It is raw.
Experimental result：Testing sample solution has violet precipitation to produce.
Comparative example 3：Tablet (Jing LC-MS are checked, and this product does not contain sulfonylureas chemical composition)
2, sample is taken, it is finely ground, in putting 10mL tool plug test tubes, 6mL 0.01mol/LNaOH solution is added, screw, shake
2min stands 2min, and supernatant liquid filtering takes 1mL filtrates and adds 0.25mL0.025mol/LCuSO4Solution, solution has blue precipitate
Produce.
Experimental result：Testing sample solution has blue precipitate to produce.
Comparative example 4：Tablet (Jing LC-MS are checked, this product chemical composition containing sulfonylureas)
Testing sample 2 is taken, in putting 10mL tool plug test tubes, 4mL 0.01mol/LNaOH solution is added, 2min is shaken, it is quiet
2min is put, supernatant liquid filtering takes 1mL filtrates and adds 0.25mL 0.01mol/LCuSO4Solution, solution has white precipitate to produce.
Experimental result：Testing sample solution has white precipitate to produce.
Comparative example 5：Granule (Jing LC-MS are checked, this product chemical composition containing sulfonylureas)
Take testing sample 1 to wrap, in putting 10mL tool plug test tubes, add 6mL 0.01mol/LNaOH solution, shake 2min, it is quiet
2min is put, supernatant liquid filtering takes 1mL filtrates and adds 0.25mL 0.001mol/LCuSO4Solution, solution is produced without precipitation.
Experimental result：Testing sample solution is produced without precipitation.
As a result it is as shown in table 2 below:
Explanation：Above-mentioned contrast test shows that NaOH solution concentration is more than or less than 0.001-1mol/L, CuSO4Test solution is dense
Degree is more than or less than 0.004-0.006mol/L, disturbed condition can all occurs, and to detection band error is carried out, and causes result to be difficult to judge
Or there is false positive.
It is described on end, whether sulfonylurea drugs can be contained according to precipitation reaction judgement sample using 2 steps using this method,
Extract used, reaction test solution are common chemical reagent, and very safe, easy to operate, analysis cost is low.And react
Sensitive, specificity is strong, and phenomenon is obvious, it is not necessary to be equipped with instrument, it is adaptable to field quick detection.
The preferred embodiments of the present invention are the foregoing is only, the scope of the claims of the present invention, every utilization is not thereby limited
The equivalent structure transformation that present specification is made, or other related technical fields are directly or indirectly used in, together
Reason is included within the scope of the present invention.
Claims (3)
1. a kind of method for quick of sulfonylureas chemical composition, it is characterised in that step is as follows：
1) extract：Chinese patent drug to be measured or appropriate health food are taken, equivalent to 1 oral dose, as test sample, finely ground or pressure
It is broken, in being put into tool plug test tube, 2-8mL 0.001-0.1mol/L NaOH solutions are added, 1-5min is shaken, 1-4min is stood, take
Supernatant liquid filtering, collects filtrate as test liquid A；
2) reacted：0.23-0.30mL 0.005mol/L CuSO are added dropwise in test liquid A4Observation phenomenon in test solution, 1min；
3) result differentiates：In 1min, if test liquid A occurs without white or light blue precipitation, can determine whether to be not added with test sample
Sulfonylureas chemical composition, in 1min, if occurring white or light blue precipitation in test liquid A, can determine whether to add sulphur in test sample
Ureas chemical composition.
2. the method for quick of sulfonylureas chemical composition according to claim 1, it is characterised in that：Above-mentioned steps 2) in
The concentration of the NaOH solution is preferably 0.01mol/L.
3. the method for quick of sulfonylureas chemical composition according to claim 1, it is characterised in that：Above-mentioned steps 2)
In, CuSO is added dropwise in test liquid A4It is not required to be shaken after test solution.
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