CN103954608B - A kind of identify the method whether adding pioglitazone or rosiglitazone in blood-sugar lowering tcm drug - Google Patents
A kind of identify the method whether adding pioglitazone or rosiglitazone in blood-sugar lowering tcm drug Download PDFInfo
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- CN103954608B CN103954608B CN201410211927.XA CN201410211927A CN103954608B CN 103954608 B CN103954608 B CN 103954608B CN 201410211927 A CN201410211927 A CN 201410211927A CN 103954608 B CN103954608 B CN 103954608B
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- rosiglitazone
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- YASAKCUCGLMORW-UHFFFAOYSA-N Rosiglitazone Chemical compound C=1C=CC=NC=1N(C)CCOC(C=C1)=CC=C1CC1SC(=O)NC1=O YASAKCUCGLMORW-UHFFFAOYSA-N 0.000 title claims abstract description 172
- HYAFETHFCAUJAY-UHFFFAOYSA-N pioglitazone Chemical compound N1=CC(CC)=CC=C1CCOC(C=C1)=CC=C1CC1C(=O)NC(=O)S1 HYAFETHFCAUJAY-UHFFFAOYSA-N 0.000 title claims abstract description 164
- 239000003814 drug Substances 0.000 title claims abstract description 160
- 229940079593 drug Drugs 0.000 title claims abstract description 142
- 229960004586 rosiglitazone Drugs 0.000 title claims abstract description 86
- 229960005095 pioglitazone Drugs 0.000 title claims abstract description 82
- 238000000034 method Methods 0.000 title claims abstract description 42
- 238000001228 spectrum Methods 0.000 claims abstract description 47
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 claims abstract description 38
- 230000003287 optical effect Effects 0.000 claims abstract description 30
- 238000004809 thin layer chromatography Methods 0.000 claims abstract description 9
- 238000001069 Raman spectroscopy Methods 0.000 claims description 82
- 239000012744 reinforcing agent Substances 0.000 claims description 17
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 13
- 229910052709 silver Inorganic materials 0.000 claims description 10
- 239000004332 silver Substances 0.000 claims description 10
- 150000002576 ketones Chemical class 0.000 claims description 9
- 238000012797 qualification Methods 0.000 claims description 9
- 230000010354 integration Effects 0.000 claims description 6
- 230000002035 prolonged effect Effects 0.000 claims description 6
- 239000000956 alloy Substances 0.000 claims description 5
- 229910045601 alloy Inorganic materials 0.000 claims description 5
- 238000012937 correction Methods 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- PQTCMBYFWMFIGM-UHFFFAOYSA-N gold silver Chemical compound [Ag].[Au] PQTCMBYFWMFIGM-UHFFFAOYSA-N 0.000 claims description 4
- 238000001237 Raman spectrum Methods 0.000 claims description 2
- 238000012360 testing method Methods 0.000 abstract description 5
- 239000000126 substance Substances 0.000 description 45
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 24
- GHUUBYQTCDQWRA-UHFFFAOYSA-N Pioglitazone hydrochloride Chemical compound Cl.N1=CC(CC)=CC=C1CCOC(C=C1)=CC=C1CC1C(=O)NC(=O)S1 GHUUBYQTCDQWRA-UHFFFAOYSA-N 0.000 description 24
- 229960002827 pioglitazone hydrochloride Drugs 0.000 description 24
- 229960003271 rosiglitazone maleate Drugs 0.000 description 20
- SUFUKZSWUHZXAV-BTJKTKAUSA-N rosiglitazone maleate Chemical compound [H+].[H+].[O-]C(=O)\C=C/C([O-])=O.C=1C=CC=NC=1N(C)CCOC(C=C1)=CC=C1CC1SC(=O)NC1=O SUFUKZSWUHZXAV-BTJKTKAUSA-N 0.000 description 20
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 20
- 239000008280 blood Substances 0.000 description 16
- 210000004369 blood Anatomy 0.000 description 16
- 230000001360 synchronised effect Effects 0.000 description 14
- 238000001514 detection method Methods 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000008279 sol Substances 0.000 description 7
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 6
- 230000008859 change Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- GLYLMXARZJNUEY-UHFFFAOYSA-N dichloromethane;methanol;hydrate Chemical compound O.OC.ClCCl GLYLMXARZJNUEY-UHFFFAOYSA-N 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000004128 high performance liquid chromatography Methods 0.000 description 4
- 238000004895 liquid chromatography mass spectrometry Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000013558 reference substance Substances 0.000 description 4
- 239000000741 silica gel Substances 0.000 description 4
- 229910002027 silica gel Inorganic materials 0.000 description 4
- 229910001961 silver nitrate Inorganic materials 0.000 description 4
- 239000001509 sodium citrate Substances 0.000 description 4
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 4
- 229940038773 trisodium citrate Drugs 0.000 description 4
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 3
- 239000011976 maleic acid Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 3
- LFDGRWDETVOGDT-UHFFFAOYSA-N 1h-pyrrole;hydrochloride Chemical compound Cl.C=1C=CNC=1 LFDGRWDETVOGDT-UHFFFAOYSA-N 0.000 description 2
- 241000208340 Araliaceae Species 0.000 description 2
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 2
- 235000003140 Panax quinquefolius Nutrition 0.000 description 2
- 241001620634 Roger Species 0.000 description 2
- 238000010923 batch production Methods 0.000 description 2
- 235000008434 ginseng Nutrition 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 206010008190 Cerebrovascular accident Diseases 0.000 description 1
- 208000013016 Hypoglycemia Diseases 0.000 description 1
- 208000006011 Stroke Diseases 0.000 description 1
- 229940127003 anti-diabetic drug Drugs 0.000 description 1
- 239000003472 antidiabetic agent Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
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- 238000013461 design Methods 0.000 description 1
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- 230000000857 drug effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002218 hypoglycaemic effect Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
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- 208000010125 myocardial infarction Diseases 0.000 description 1
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- 230000009466 transformation Effects 0.000 description 1
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- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
A kind of identify the method whether adding pioglitazone or rosiglitazone in blood-sugar lowering tcm drug, the method includes that taking blood-sugar lowering tcm drug to be checked carries out thin layer chromatography, doubtful speckle is found at the Rf value that pioglitazone is corresponding with rosiglitazone, it is characterized in that, also include three below step: 1, gather a series of one-dimensional surface enhanced raman spectroscopy of doubtful speckle, obtain the dynamic spectrum of blood-sugar lowering tcm drug to be checked, 2, dynamic optical spectrogram is carried out pretreatment, and draw the two-dimensional correlation surface enhanced raman spectroscopy figure obtaining blood-sugar lowering tcm drug to be checked；3, according to the two-dimensional correlation surface enhanced raman spectroscopy figure of blood-sugar lowering tcm drug to be checked, it is judged that whether blood-sugar lowering tcm drug to be checked has pioglitazone and rosiglitazone.According to technical scheme provided by the present invention, it is possible to whether blood-sugar lowering tcm drug adding pioglitazone or rosiglitazone quickly differentiates, testing result accurately and reliably, low cost, easy to operate.
Description
Technical field
The present invention relates to a kind of method identified and whether add pioglitazone or rosiglitazone in blood-sugar lowering tcm drug, belong to
In medicine analysis technical field.
Background technology
In recent years, cheap, drug effect, in order to seek great number interests, is added in blood-sugar lowering tcm drug in some pharmaceutical factories
Suitable blood sugar lowering Western medicine pioglitazone hydrochloride, rosiglitazone maleate or the mixture of the two, these blood sugar lowering west
Although medicine also can play blood sugar reducing function, but side effect is relatively big, especially rosiglitazone maleate, because it can be big
Width increases user's heart attack and the probability of apoplexy, and food and drug administration is in 2011
This product of undercarriage comprehensively.If patient's long-term taking with the addition of these blood sugar lowering Western medicine blood-sugar lowering tcm drugs, not only can draw
Play the multiple untoward reaction, even entail dangers to such as hypoglycemia sick, produce serious consequence.Therefore, fall is identified
Whether saccharide Chinese medicine with the addition of pioglitazone or rosiglitazone, an important process of Shi Yaojian department.
Method master currently for the detection of adulterate in blood-sugar lowering tcm drug rosiglitazone maleate and pioglitazone hydrochloride
TLC, HPLC, LC-MS to be had etc..Although TLC method is simple and quick, but be only capable of in antidiabetic drug whether
Adulterated make superficial judgement, be that what composition can not be identified to doping concrete in adulterated blood-sugar lowering tcm drug,
And the method is easily affected by Chinese medicine substrate and adulterated amount and is demonstrated false positive or false-negative result.HPLC
Although with LC-MS can be to doping concrete in adulterated blood-sugar lowering tcm drug pioglitazone or rosiglitazone or
The mixture of the two judges, but analytical cycle length, experiment condition are harsh, need specific chromatographic column,
Whether flowing equal, testing cost is higher, especially add in Yao Jian department needs at the scene to blood-sugar lowering tcm drug
Add pioglitazone hydrochloride or rosiglitazone maleate or time both has interpolation make detection and judge, these sides
Method will be difficult to be suitable for.
Summary of the invention
It is an object of the invention to provide whether a kind of qualification adds pioglitazone or rosiglitazone in blood-sugar lowering tcm drug
Method, to solve the problems referred to above.
To achieve these goals, the technical solution adopted in the present invention is:
Adding pioglitazone or the authentication method of rosiglitazone in a kind of blood-sugar lowering tcm drug, the method includes taking to be checked
Blood-sugar lowering tcm drug carries out thin layer chromatography, finds doubtful speckle at the Rf value that pioglitazone is corresponding with rosiglitazone,
It is characterized in that, also include three below step:
Step one: the collection of dynamic optical spectrogram
Take surface reinforcing agent point on doubtful speckle, use Raman spectrometer, choose the laser pair of some strength
Doubtful speckle prolonged exposure carries out perturbation, and gathers a series of one-dimensional surface enhanced Raman light of doubtful speckle
Spectrum, obtains the dynamic spectrum of blood-sugar lowering tcm drug to be checked, the phase time of integration of every one-dimensional surface enhanced raman spectroscopy
With, some strength is any number between 100mW～200mW, surface reinforcing agent be aurosol, silver molten
Glue or gold silver rubber alloy, the point sample amount of surface reinforcing agent is 2 μ L～10 μ L；
Step 2: the drafting of two-dimensional correlation surface enhanced raman spectroscopy figure
Dynamic optical spectrogram is carried out pretreatment, including choosing 300cm-1～1700cm-1Spectral coverage, employing Sgolay
Method carries out smooth and uses airPLS method to carry out baseline correction, obtains the pretreatment Raman light of blood-sugar lowering tcm drug to be checked
Spectrogram, according to pretreatment Raman spectrogram, drafting obtains the two-dimensional correlation surface enhanced of blood-sugar lowering tcm drug to be checked and draws
Graceful spectrogram；
Step 3: to whether adding pioglitazone or rosiglitazone is identified
Two-dimensional correlation surface enhanced raman spectroscopy figure according to blood-sugar lowering tcm drug to be checked, when containing and pyrrole in this spectrogram
The peak position that goes out of the relevant peaks of lattice row ketone differs-w～the relevant peaks of w wave number, then judge to contain in blood-sugar lowering tcm drug to be checked
There is pioglitazone, when this spectrogram differs-w～w wave number containing the peak position that goes out with the relevant peaks of rosiglitazone
Relevant peaks, then judge containing rosiglitazone in blood-sugar lowering tcm drug to be checked, when not containing and pioglitazone in this spectrogram
With rosiglitazone relevant peaks go out peak position difference-w～the relevant peaks of w wave number, then judge in blood sugar lowering to be checked
Not containing pioglitazone and rosiglitazone in medicine, w is 1cm-1～5cm-1Between any number, pyrrole lattice arrange
The peak position that goes out of the relevant peaks of ketone is set to: 414cm-1,430cm-1,475cm-1,824cm-1, the relevant peaks of rosiglitazone
The peak position that goes out be set to: 739cm-1,1255cm-1,1329cm-1。
Present invention also offers such technical scheme:
Whether adding the authentication method of pioglitazone or rosiglitazone in a kind of blood-sugar lowering tcm drug, the method includes:
Take blood-sugar lowering tcm drug to be checked and carry out thin layer chromatography, find doubtful at the Rf value that pioglitazone is corresponding with rosiglitazone
Like speckle, it is characterised in that also include three below step:
Step one: the collection of dynamic optical spectrogram
After blood-sugar lowering tcm drug to be checked, pioglitazone standard substance and rosiglitazone standard substance are carried out thin layer chromatography,
Doubtful speckle, pioglitazone and three speckles of rosiglitazone are found on lamellae,
Take surface reinforcing agent respectively o'clock on three speckles, use Raman spectrometer, choose swashing of some strength
Light carries out perturbation respectively to three speckle prolonged exposures, and gathers a series of one-dimensional surface of three speckles respectively
Strengthen Raman spectrum, obtain the dynamic optical spectrogram of doubtful speckle, pioglitazone and rosiglitazone, each speckle
Time of integration of all one-dimensional surface enhanced raman spectroscopy the most identical, some strength is 100mW～200mW
Between any number, surface reinforcing agent is aurosol, silver sol or gold silver rubber alloy, the point of surface reinforcing agent
Sample amount is 2 μ L～10 μ L；
Step 2: the drafting of two-dimensional correlation surface enhanced raman spectroscopy figure
Respectively the dynamic optical spectrogram of blood-sugar lowering tcm drug to be checked, pioglitazone standard substance and rosiglitazone standard substance is entered
Row pretreatment, including choosing 300cm-1～1700cm-1Spectral coverage, employing Sgolay method carry out smooth and use
AirPLS method carries out baseline correction, obtains blood-sugar lowering tcm drug to be checked, pioglitazone standard substance and rosiglitazone standard
The pretreatment Raman spectrogram of product, according to pretreatment Raman spectrogram, draws the two-dimensional phase obtaining three respectively
Close surface enhanced raman spectroscopy figure；
Step 3: the analysis of two-dimensional correlation surface enhanced raman spectroscopy figure and judgement
By the two-dimensional correlation surface enhanced raman spectroscopy figure of blood-sugar lowering tcm drug to be checked respectively with pioglitazone standard substance with
And the two-dimensional correlation surface enhanced raman spectroscopy figure of rosiglitazone standard substance compares, when blood-sugar lowering tcm drug to be checked
Two-dimensional correlation surface enhanced raman spectroscopy figure in containing with the relevant peaks of pioglitazone standard substance go out peak position
Difference-w～the relevant peaks of w wave number, then judge containing pioglitazone in blood-sugar lowering tcm drug to be checked, when in blood sugar lowering to be checked
Contain the relevant peaks with rosiglitazone standard substance in the two-dimensional correlation surface enhanced raman spectroscopy figure of medicine goes out peak position
Put difference-w～the relevant peaks of w wave number, then judge containing rosiglitazone in blood-sugar lowering tcm drug to be checked, when blood sugar lowering to be checked
The two-dimensional correlation surface enhanced raman spectroscopy figure of Chinese medicine does not contains and pioglitazone standard substance and rosiglitazone mark
Quasi-product relevant peaks go out peak position difference-w～the relevant peaks of w wave number, then judge in blood-sugar lowering tcm drug to be checked not
Containing pioglitazone and rosiglitazone, w is 1cm-1～5cm-1Between any number.
The pioglitazone standard substance that are further characterized by of technical scheme are pioglitazone hydrochloride mark
Quasi-product, rosiglitazone standard substance are rosiglitazone maleate standard substance.
The some strength that is further characterized by of the technical scheme of the invention described above is 200mW.
The technical scheme of the invention described above be further characterized by two-dimensional correlation surface enhanced raman spectroscopy figure
For synchronizing spectrum.
The technical scheme of the invention described above be further characterized by the laser laser by Raman spectrometer self
Light source provides.
The surface reinforcing agent that is further characterized by of the technical scheme of the invention described above is nano silver colloidal sol.
The point sample amount being further characterized by surface reinforcing agent of the technical scheme of the invention described above is
4 μ L～6 μ L.
The w that is further characterized by of the technical scheme of the invention described above is 5cm-1。
Compared with background technology, advantage and the good effect of technical scheme are as follows:
1. can be to whether blood-sugar lowering tcm drug adding pioglitazone or rosiglitazone quickly differentiates
Technical scheme uses laser to carrying out perturbation at doubtful speckle, uses Raman spectrometer detection
Obtain the two-dimensional correlation surface enhanced raman spectroscopy figure of blood-sugar lowering tcm drug to be checked, by judging that this dimension relevant surfaces increases
Whether strong Raman spectrogram contains with pioglitazone or rosiglitazone go out identical automatic peak, peak position or phase
Guan Feng, can realize whether adding pioglitazone in blood-sugar lowering tcm drug to be checked or rosiglitazone judges, with
HPLC with LC-MS compares, it is not necessary to harsh experiment condition and the work of complicated sample pre-treatments,
Quickly identify and whether blood-sugar lowering tcm drug to be checked adds pioglitazone or rosiglitazone.
2. characteristic is strong, and testing result is accurately and reliably
Owing to Raman spectroscopy has extremely strong characteristic and the lowest, therefore to the content requirement of detection material
The qualification result that drawn according to technical scheme accurately and reliably, compared with TLC, it is to avoid false sun
Property or the appearance of false negative result, it is possible to foundation and the guidance of science are provided for the staff of Yao Jian department.
3. low cost, easy to operate
Technical scheme uses lamellae and Raman spectrometer to implement, and equipment and experimental situation are wanted
Ask simple, low cost, easy to operate, when the Raman spectrometer used is portable or during hand-held, permissible
Realize whether blood-sugar lowering tcm drug adding rosiglitazone maleate and pioglitazone hydrochloride carries out on-the-spot quickly mirror
Fixed.
Accompanying drawing explanation
Fig. 1 is technical scheme flow chart in embodiment one；
Fig. 2 is Raman spectrogram after the pretreatment of blood-sugar lowering tcm drug to be checked in embodiment one；
Fig. 3 is Raman spectrogram after the pretreatment of pioglitazone hydrochloride standard substance in embodiment one；
Fig. 4 is Raman spectrogram after the pretreatment of rosiglitazone maleate standard substance in embodiment one；
Fig. 5 is that the two-dimensional correlation surface-enhanced Raman synchronous spectrum of blood-sugar lowering tcm drug to be checked in embodiment one is divided into
The synchronization correlation spectrum obtained after three sections；
Fig. 6 is the two-dimensional correlation surface-enhanced Raman synchronous spectrum of pioglitazone hydrochloride standard substance in embodiment one
The synchronization correlation spectrum obtained after being divided into three sections；
Fig. 7 is the two-dimensional correlation surface-enhanced Raman synchronizable optical of rosiglitazone maleate standard substance in embodiment one
The synchronization correlation spectrum that spectrum obtains after being divided into three sections；
Fig. 8 is technical scheme flow chart in embodiment two；
Fig. 9 is Raman spectrogram after the pretreatment of blood-sugar lowering tcm drug to be checked in embodiment two；
Figure 10 is that the two-dimensional correlation surface-enhanced Raman synchronous spectrum of blood-sugar lowering tcm drug to be checked in embodiment two is divided into
The synchronization correlation spectrum obtained after three sections；
Figure 11 is Raman spectrogram after the pretreatment of blood sugar lowering sample to be checked in embodiment three；And
Figure 12 is that the two-dimensional correlation surface-enhanced Raman synchronous spectrum of blood sugar lowering sample to be checked in embodiment three is divided into
The synchronization correlation spectrum obtained after three sections.
Detailed description of the invention
Below in conjunction with accompanying drawing, to the detection method whether adding analog in medicine involved in the present invention
It is described further.
Concept explanation involved in following example:
Synchronize spectrum: sign is the direction of change in signal strength at two wave numbers and collaborative degree, when two are moved
State change homophase (anti-phase), is worth for just (bearing)；When dynamically change is orthogonal, value is zero.
Relevant peaks: diagonal and off-diagonal region all there will be, including automatic peak and intersection peak.
Automatically peak: the relevant peaks being positioned on leading diagonal, expression is the same wave number under same disturbance
Relevant spectrum peak, the sensitivity that its intensity reflection system is externally disturbed.
Intersection peak: the intersection peak being positioned on off-diagonal, represents the synchronization change at the peak being positioned at different wave number,
Represent that the change at two peaks has common mechanism and origin.
<embodiment one>
One, instrument and sample
(1) instrument: BWS415-785H type Portable Raman spectrometer (Bi Da Imtech of the U.S.), swashs
Send out wavelength 785nm；
(2) prepared by silver sol: take silver nitrate (AgNO3) 17mg add secondary deionized water 100ml dissolve,
Adding the trisodium citrate 1.6ml of 1%, put with high fire heating 6min in microwave oven, solution is celadon, cold
But to room temperature, add water at scale, standby.
(3) blood-sugar lowering tcm drug solution to be checked and the preparation of reference substance solution: take the blood sugar lowering that A pharmaceutical factory batch produces
Chinese medicine, as blood-sugar lowering tcm drug to be checked, takes blood-sugar lowering tcm drug to be checked, pioglitazone hydrochloride standard substance and Malaysia respectively
Acid rosiglitazone standard substance are appropriate, make the blood-sugar lowering tcm drug to be checked of 1mol/L, pioglitazone hydrochloride standard substance,
And the methanol solution of rosiglitazone maleate standard substance.
Two, blood-sugar lowering tcm drug to be checked is detected
Fig. 1 is technical scheme flow chart in embodiment one.
As it is shown in figure 1, in the present embodiment one, measure and whether this blood-sugar lowering tcm drug to be checked add hydrochloric acid pyrrole lattice
Row ketone or rosiglitazone maleate, including three below step:
Step one (S1): the collection of dynamic optical spectrogram
Take 1 μ l blood-sugar lowering tcm drug to be checked, pioglitazone hydrochloride standard substance and the methanol of rosiglitazone maleate standard substance
Solution is put respectively on silica gel thin-layer plate (hereinafter referred to as lamellae), through methylene chloride-methanol-water (volume ratio
After 8:2:0.2) launching, taking-up volatilizes, and inspects pioglitazone hydrochloride standard substance and horse under uviol lamp 254nm
Carry out sour rosiglitazone standard substance speckle displacement on lamellae, be respectively labeled as pioglitazone and rosiglitazone,
Inspect in the chromatographic bands of this blood-sugar lowering tcm drug to be checked with pioglitazone hydrochloride standard substance and rosiglitazone maleate mark
Quasi-product relevant position there is also chromatograph speckle, this chromatograph speckle is labeled as doubtful speckle, takes 5 μ l silver sols,
Drip respectively on doubtful speckle, pioglitazone and three speckles of rosiglitazone.
The laser intensity of Raman spectrometer is adjusted to 200mW, uses the LASER Light Source of this Raman spectrometer self
The laser of the 200mW provided, carries out perturbation to prolonged exposure at doubtful speckle, gathers at doubtful speckle simultaneously
A series of surface enhanced raman spectroscopy, be 5s, gained the time of integration of every surface enhanced raman spectroscopy
A series of surface enhanced raman spectroscopy are the dynamic spectrum of blood-sugar lowering tcm drug to be checked.During spectra collection,
Keeping laser intensity constant, illuminated laser spot is constant.
With reference to said method, respectively obtain pioglitazone hydrochloride standard substance and rosiglitazone maleate standard substance
Dynamic spectrum.
Step 2 (S2): the drafting of two-dimensional correlation surface enhanced raman spectroscopy figure
Fig. 2 is Raman spectrogram after the pretreatment of blood-sugar lowering tcm drug to be checked in embodiment one.
Fig. 3 is Raman spectrogram after the pretreatment of pioglitazone hydrochloride standard substance in embodiment one.
Fig. 4 is Raman spectrogram after the pretreatment of rosiglitazone maleate standard substance in embodiment one.
Utilize Matlab7.6 software that the dynamic optical spectrogram of this blood-sugar lowering tcm drug to be checked is carried out pretreatment, including spectral coverage
Choose (300cm-1～1700cm-1), smooth (Sgolay method) and baseline correction (airPLS method), obtain as
The pretreatment Raman spectrogram of this blood-sugar lowering tcm drug to be checked shown in Fig. 2, with reference to pretreatment aforesaid operations, respectively
Obtain after the pretreatment of pioglitazone hydrochloride standard substance as shown in Figure 3 Raman spectrogram and such as Fig. 4 institute
Raman spectrogram after the pretreatment of the rosiglitazone maleate standard substance shown.
Fig. 5 is that the two-dimensional correlation surface-enhanced Raman synchronous spectrum of blood-sugar lowering tcm drug to be checked in embodiment one is divided into
The synchronization correlation spectrum obtained after three sections.
Fig. 6 is the two-dimensional correlation surface-enhanced Raman synchronous spectrum of pioglitazone hydrochloride standard substance in embodiment one
The synchronization correlation spectrum obtained after being divided into three sections.
Fig. 7 is the two-dimensional correlation surface-enhanced Raman synchronizable optical of rosiglitazone maleate standard substance in embodiment one
The synchronization correlation spectrum that spectrum obtains after being divided into three sections.
By 2Dshiger version1.3 software, software dynamic spectrum is set to averaged spectrum, contour parameter
It is 8, the pretreatment Raman spectrogram of blood-sugar lowering tcm drug to be checked is processed, draw and obtain this blood-sugar lowering tcm drug to be checked
Two-dimensional correlation surface-enhanced Raman synchronizable optical spectrogram, by the two-dimensional correlation surface of pioglitazone hydrochloride standard substance
Strengthen Raman synchronous spectrum (300cm-1～1700cm-1) it is divided into 300cm as shown in Figure 5-1～500cm-1,
500cm-1～1000cm-1, and 1000cm-1～1700cm-1Three sections, wherein 5-a is 1000cm-1
～1700cm-1Section, 5-b is 500cm-1～1000cm-1Section, 5-c is 300cm-1～500cm-1Section.
With reference to above-mentioned method for drafting and partition method, draw respectively and obtain pioglitazone hydrochloride standard substance and Malaysia
The acid two-dimensional correlation surface-enhanced Raman synchronizable optical spectrogram of rosiglitazone standard substance also carries out subregion, obtains such as Fig. 6
The two-dimensional correlation surface-enhanced Raman synchronous spectrum of shown pioglitazone hydrochloride and maleic acid as shown in Figure 7
Two-dimensional correlation surface-enhanced Raman synchronous spectrum, as shown in Figure 6,6-a is the two of pioglitazone hydrochloride standard substance
Dimension relevant surfaces strengthens 1000cm in Raman synchronous spectrum-1～1700cm-1Section figure, 6-b is 500cm-1
～1000cm-1Section, 6-c is 300cm-1～500cm-1Section；As it is shown in fig. 7,7-a is maleic acid Roger
1000cm in the two-dimensional correlation surface-enhanced Raman synchronous spectrum of row ketone standard substance-1～1700cm-1Section figure, 7-b
For 500cm-1～1000cm-1Section, 7-c is 300cm-1～500cm-1Section.
Step 3 (S3): to whether adding pioglitazone or rosiglitazone is identified
By the two-dimensional correlation surface enhanced raman spectroscopy figure of blood-sugar lowering tcm drug to be checked respectively with pioglitazone standard substance with
And the two-dimensional correlation surface enhanced raman spectroscopy figure of rosiglitazone standard substance compares, when blood-sugar lowering tcm drug to be checked
Two-dimensional correlation surface enhanced raman spectroscopy figure in containing with the relevant peaks of pioglitazone standard substance go out peak position
Difference-w～the relevant peaks of w wave number, then judge containing pioglitazone in blood-sugar lowering tcm drug to be checked, when in blood sugar lowering to be checked
Contain the relevant peaks with rosiglitazone standard substance in the two-dimensional correlation surface enhanced raman spectroscopy figure of medicine goes out peak position
Put difference-w～the relevant peaks of w wave number, then judge containing rosiglitazone in blood-sugar lowering tcm drug to be checked, when blood sugar lowering to be checked
The two-dimensional correlation surface enhanced raman spectroscopy figure of Chinese medicine does not contains and pioglitazone standard substance and rosiglitazone mark
Quasi-product relevant peaks go out peak position difference-w～the relevant peaks of w wave number, then judge in blood-sugar lowering tcm drug to be checked not
Containing pioglitazone and rosiglitazone, w is 5cm-1。
Comparison Fig. 5,6,7, to whether this blood-sugar lowering tcm drug to be checked adds pioglitazone or rosiglitazone or the two
Interpolation is all had to be analyzed.
Comparison Fig. 5-a, Fig. 6-a, Fig. 7-a, at 1000cm-1～1700cm-1Section, in blood-sugar lowering tcm drug to be checked
Containing with the relevant peaks of rosiglitazone go out the automatic peak 1255cm that peak position is identical-1And 1329cm-1。
Comparison Fig. 5-b, Fig. 6-b, Fig. 7-b, at 500cm-1～1000cm-1Section, in blood-sugar lowering tcm drug to be checked
Containing with the relevant peaks of pioglitazone go out the automatic peak 627cm that peak position is identical-1, possibly together with rosiglitazone
Relevant peaks go out the automatic peak 739cm that peak position is identical-1。
Comparison Fig. 5-c, Fig. 6-c, Fig. 7-c, at 300cm-1～500cm-1Section, contains in blood-sugar lowering tcm drug to be checked
There is 475cm-1Locate automatic peak, and 414cm-1With 430cm-1The orthogonal peak at place, all with the phase of pioglitazone
Guan Feng to go out peak situation identical.
Comprehensive 1000cm-1～1700cm-1、500cm-1～1000cm-1And 300cm-1～500cm-1Three districts
, there is 414cm in the spectrogram of blood-sugar lowering tcm drug to be checked in section-1,430cm-1,475cm-1,824cm-1Place's relevant peaks, says
Bright containing pioglitazone hydrochloride, 739cm occurs-1,1255cm-1,1329cm-1Place's relevant peaks, illustrates containing Malaysia
Acid rosiglitazone.
According to above analysis result, illustrate that the blood-sugar lowering tcm drug of this pharmaceutical factory this batch production is mixed with pioglitazone and sieve
Lattice row ketone.
<embodiment two>
One, instrument and sample
(1) instrument: BWS415-785H type Portable Raman spectrometer (Bi Da Imtech of the U.S.), swashs
Send out wavelength 785nm；
(2) prepared by silver sol: take silver nitrate (AgNO3) 17mg add secondary deionized water 100ml dissolve,
Adding the trisodium citrate 1.6ml of 1%, put with high fire heating 6min in microwave oven, solution is celadon, cold
But to room temperature, add water at scale, standby.
(3) blood-sugar lowering tcm drug solution to be checked and the preparation of reference substance solution: take the blood sugar lowering that B pharmaceutical factory batch produces
Chinese medicine, as blood-sugar lowering tcm drug to be checked, makes methanol (analytical pure) solution of the blood-sugar lowering tcm drug to be checked of 1mol/L.
Two, blood-sugar lowering tcm drug to be checked is detected
Fig. 8 is technical scheme flow chart in embodiment two.
As shown in Figure 8, in the present embodiment two, measure and whether this blood-sugar lowering tcm drug to be checked adds hydrochloric acid pyrrole lattice
Row ketone or rosiglitazone maleate, the method includes: take the methanol solution point of 1 μ l blood-sugar lowering tcm drug to be checked in silica gel
On lamellae (hereinafter referred to as lamellae), after methylene chloride-methanol-water (8:2:0.2) launches, taking-up is waved
Dry, inspect under uviol lamp 254nm, find doubtful at the Rf value that pioglitazone or rosiglitazone are corresponding
Speckle (Rf value is 0.9), also includes three below step:
Step one (S1 '): the collection of dynamic optical spectrogram
Take 5 μ l silver sols and drip on doubtful speckle, the laser intensity of Raman spectrometer is adjusted to 200mW, adopts
Launch laser with the LASER Light Source of this Raman spectrometer self, doubtful speckle prolonged exposure is carried out perturbation, with
Time gather a series of surface enhanced raman spectroscopy of doubtful speckle, obtain the dynamic spectrum of this blood-sugar lowering tcm drug to be checked,
The time of integration of every surface enhanced raman spectroscopy is 5s, during spectra collection, keeps laser intensity
Constant, illuminated laser spot is constant.
Step 2 (S2 '): the drafting of two-dimensional correlation surface enhanced raman spectroscopy figure
Fig. 9 is Raman spectrogram after the pretreatment of blood-sugar lowering tcm drug to be checked in embodiment two.
Figure 10 is that the two-dimensional correlation surface-enhanced Raman synchronous spectrum of blood-sugar lowering tcm drug to be checked in embodiment two is divided into
The synchronization correlation spectrum obtained after three sections.
Utilize Matlab7.6 software that the dynamic optical spectrogram of this blood-sugar lowering tcm drug to be checked is carried out pretreatment, including spectral coverage
Choose (300cm-1～1700cm-1), smooth (Sgolay method) and baseline correction (airPLS method), obtain as
The pretreatment Raman spectrogram of this blood-sugar lowering tcm drug to be checked shown in Fig. 9.
By 2Dshiger version1.3 software, software dynamic spectrum is set to averaged spectrum, contour parameter
It is 8, the pretreatment Raman spectrogram of blood-sugar lowering tcm drug to be checked is processed, draw and obtain as shown in Figure 10
The two-dimensional correlation surface-enhanced Raman synchronizable optical spectrogram of this blood-sugar lowering tcm drug to be checked, by the two of this blood-sugar lowering tcm drug to be checked
Dimension relevant surfaces strengthens Raman synchronous spectrum (300cm-1～1700cm-1) be divided into as shown in Figure 10
300cm-1～500cm-1,500cm-1～1000cm-1, and 1000cm-1～1700cm-1Three sections, wherein 10-a
For 1000cm-1～1700cm-1Section, 10-b is 500cm-1～1000cm-1Section, 10-c is 300cm-1
～500cm-1Section.
Step 3 (S3 '): to whether adding pioglitazone or rosiglitazone is identified
Two-dimensional correlation surface-enhanced Raman synchronizable optical spectrogram according to this blood-sugar lowering tcm drug to be checked, when containing in this spectrogram
The peak position that goes out having the relevant peaks with pioglitazone differs-w～the relevant peaks of w wave number, then judge in blood sugar lowering to be checked
Containing pioglitazone in medicine, when the peak position that goes out containing the relevant peaks with rosiglitazone in this spectrogram differs-w～w
The relevant peaks of wave number, then judge containing rosiglitazone in blood-sugar lowering tcm drug to be checked, when not containing and pyrrole in this spectrogram
Lattice row ketone and rosiglitazone relevant peaks go out peak position difference-w～the relevant peaks of w wave number, then judge to be checked
Not containing pioglitazone and rosiglitazone in blood-sugar lowering tcm drug, w is 5cm-1, the relevant peaks of pioglitazone go out peak
Position is: 414cm-1,430cm-1,475cm-1,824cm-1, the peak position that goes out of the relevant peaks of rosiglitazone is set to:
739cm-1,1255cm-1,1329cm-1。
From Figure 10-a, 10-b, 10-c, the two-dimensional correlation table of the blood-sugar lowering tcm drug to be checked that the present embodiment is provided
Face strengthens in Raman synchronizable optical spectrogram at 414cm-1,430cm-1,475cm-1,824cm-1The existence relevant peaks at place,
Illustrate that the blood-sugar lowering tcm drug of this pharmaceutical factory this batch production is mixed with pioglitazone.
<embodiment three>
One, instrument and sample
(1) instrument: BWS415-785H type Portable Raman spectrometer (Bi Da Imtech of the U.S.), swashs
Send out wavelength 785nm；
(2) prepared by silver sol: take silver nitrate (AgNO3) 17mg add secondary deionized water 100ml dissolve,
Adding the trisodium citrate 1.6ml of 1%, put with high fire heating 6min in microwave oven, solution is celadon, cold
But to room temperature, add water at scale, standby.
(3) blood-sugar lowering tcm drug solution to be checked and the preparation of reference substance solution: take the blood sugar lowering that C pharmaceutical factory batch produces
Chinese medicine, as blood-sugar lowering tcm drug to be checked, makes methanol (analytical pure) solution of the blood-sugar lowering tcm drug to be checked of 1mol/L.
Two, blood-sugar lowering tcm drug to be checked is detected
In the present embodiment three, take the methanol solution point of 1 μ l blood-sugar lowering tcm drug to be checked in silica gel thin-layer plate (letter below
Claim lamellae) on, after methylene chloride-methanol-water (8:2:0.2) launches, taking-up volatilizes, in uviol lamp 254nm
Under inspect, at the Rf value that pioglitazone hydrochloride or rosiglitazone maleate are corresponding, find doubtful speckle, ginseng
According to the operation of step one in embodiment two to step 3, doubtful speckle is carried out the collection of dynamic optical spectrogram, two
Dimension relevant surfaces strengthens the drafting of Raman spectrogram and to whether adding pioglitazone or rosiglitazone is carried out
Identify.
Figure 11 is Raman spectrogram after the pretreatment of blood-sugar lowering tcm drug to be checked in embodiment three；
Figure 12 is that the two-dimensional correlation surface-enhanced Raman synchronous spectrum of blood-sugar lowering tcm drug to be checked in embodiment three is divided into
The synchronization correlation spectrum obtained after three sections.
As shown in figure 11 this is obtained to be checked after dynamic optical spectrogram being carried out pretreatment by Matlab7.6 software
The pretreatment Raman spectrogram of blood-sugar lowering tcm drug, obtains such as Figure 12 institute through 2Dshiger version1.3 Software on Drawing
The two-dimensional correlation surface-enhanced Raman synchronizable optical spectrogram of this blood-sugar lowering tcm drug shown,
From Figure 12-a, 12-b, 12-c, the two-dimensional correlation table of the blood-sugar lowering tcm drug to be checked that the present embodiment is provided
Face strengthens in Raman synchronizable optical spectrogram at 739cm-1,1255cm-1,1329cm-1The existence relevant peaks at place, explanation
The blood-sugar lowering tcm drug that this batch of this pharmaceutical factory produces is mixed with rosiglitazone maleate.
<embodiment four>
One, instrument and sample
(1) instrument: BWS415-785H type Portable Raman spectrometer (Bi Da Imtech of the U.S.), swashs
Send out wavelength 785nm；
(2) prepared by silver sol: take silver nitrate (AgNO3) 17mg add secondary deionized water 100ml dissolve,
Adding the trisodium citrate 1.6ml of 1%, put with high fire heating 6min in microwave oven, solution is celadon, cold
But to room temperature, add water at scale, standby.
(3) blood-sugar lowering tcm drug solution to be checked and the preparation of reference substance solution: take the blood sugar lowering that D pharmaceutical factory batch produces
Chinese medicine, as blood-sugar lowering tcm drug to be checked, makes methanol (analytical pure) solution of the blood-sugar lowering tcm drug to be checked of 1mol/L.
Two, blood-sugar lowering tcm drug to be checked is detected
In the present embodiment four, take the methanol solution point of 1 μ l blood-sugar lowering tcm drug to be checked in silica gel thin-layer plate (letter below
Claim lamellae) on, after methylene chloride-methanol-water (8:2:0.2) launches, taking-up volatilizes, in uviol lamp 254nm
Under inspect, at the Rf value that pioglitazone hydrochloride or rosiglitazone maleate are corresponding, find doubtful speckle, ginseng
According to the operation of step one in embodiment two to step 3, doubtful speckle is carried out the collection of dynamic optical spectrogram, two
Dimension relevant surfaces strengthens the drafting of Raman spectrogram and to whether adding pioglitazone or rosiglitazone is carried out
Identify.
The pre-place of this blood-sugar lowering tcm drug to be checked is obtained after dynamic optical spectrogram being carried out pretreatment by Matlab7.6 software
Reason Raman spectrogram, obtains the two-dimensional correlation surface of this blood-sugar lowering tcm drug through 2Dshiger version1.3 Software on Drawing
Strengthening Raman synchronizable optical spectrogram, spectrogram shows, at 414cm-1,430cm-1,475cm-1,824cm-1Place does not go out
Existing relevant peaks, illustrates not contain pioglitazone, at 739cm in this blood-sugar lowering tcm drug to be checked-1,1255cm-1,1329cm-1
The most there is not relevant peaks in place, illustrates not contain rosiglitazone in this blood-sugar lowering tcm drug to be checked yet.
The effect of embodiment and effect
Compared with background technology, in the blood-sugar lowering tcm drug that above-described embodiment one to four is provided add pioglitazone or
The effect of the authentication method of rosiglitazone with good effect is:
1. can be to whether blood-sugar lowering tcm drug adding pioglitazone or rosiglitazone quickly differentiates
Technical scheme uses laser to carrying out perturbation at doubtful speckle, uses Raman spectrometer detection
Obtain the two-dimensional correlation surface enhanced raman spectroscopy figure of blood-sugar lowering tcm drug to be checked, by judging that this dimension relevant surfaces increases
Whether strong Raman spectrogram contains with pioglitazone or rosiglitazone go out identical automatic peak, peak position or phase
Guan Feng, can realize whether adding pioglitazone in blood-sugar lowering tcm drug to be checked or rosiglitazone judges, with
HPLC with LC-MS compares, it is not necessary to harsh experiment condition and the work of complicated sample pre-treatments,
Quickly identify and whether blood-sugar lowering tcm drug to be checked adds pioglitazone or rosiglitazone.
2. characteristic is strong, and testing result is accurately and reliably
Owing to Raman spectroscopy has extremely strong characteristic and the lowest, therefore to the content requirement of detection material
The qualification result that drawn according to technical scheme accurately and reliably, compared with TLC, it is to avoid false sun
Property or the appearance of false negative result, it is possible to foundation and the guidance of science are provided for the staff of Yao Jian department.
3. low cost, easy to operate
Technical scheme uses lamellae and Portable Raman spectrometer to implement, equipment and experiment
Environmental requirement is simple, and low cost is easy to operate, can be to whether adding maleic acid Roger row in blood-sugar lowering tcm drug
Ketone and pioglitazone hydrochloride carry out on-the-spot Rapid identification.
4. perturbation design is ingenious, easy to be quick, easily operated
The laser of the Raman spectrometer self needed for employing experiment is to carrying out prolonged exposure at point sample, thus produces
Heat carries out perturbation to testing sample, it is thus achieved that series dynamically SERS spectrogram, and then obtains two-dimensional correlation spectrogram.
Whole experimentation, without additional interference experiment, only need to regulate and control laser energy, it is to avoid artificial applying is micro-
Be likely to occur when disturbing measure because of temperature is too high or pH change excessive etc. caused by the shortcoming destroyed of sample system,
And simple to operate, it is easy to reappear, it is simple to medicine prison personnel carry out Site Detection.
Certainly, whether a kind of blood-sugar lowering tcm drug involved in the present invention adds the mirror of pioglitazone or rosiglitazone
Determine the content that method is not merely defined in above-described embodiment.Above content is only the base under present inventive concept
This explanation, and according to any equivalent transformation that technical scheme is made, belong to the protection of the present invention
Scope.
It addition, in above-described embodiment one to four, the laser intensity of Raman spectrometer is 200mW.The present invention
Involved laser intensity can in dynamic spectrum gatherer process ensure n.s calcination situation institute occur
Any intensity used, any number between preferably 100mW～200mW, preferably 200mW.
It addition, in above-described embodiment one to four, w is 5cm-1, technical scheme w can be selected from
1cm-1To 5cm-1Between any number, preferably 5cm-1。
It addition, in the above-described embodiments, the point sample amount of surface reinforcing agent is 5 μ L, in technical scheme
In, the point sample amount of surface reinforcing agent can be selected from any number between 2 μ L～10 μ L, preferably 4 μ L～6 μ L
Between numerical value.
It addition, in above-described embodiment one to four, select two-dimensional correlation surface-enhanced Raman synchronizable optical spectrogram
Synchronization spectrum is analyzed, and technical scheme can also be for two-dimensional correlation surface-enhanced Raman synchronizable optical
The asynchronous spectrum of spectrogram is analyzed.
It addition, in above-described embodiment one to four, the collection of dynamic spectrum be at equal intervals the time period be acquired,
Technical scheme can also is that and is incremented by according to interval time or adopts according to successively decreasing interval time
Collection, as long as ensureing that the time of integration of every spectrogram is identical.
It addition, in above-described embodiment one to four, the surface reinforcing agent used is nano silver colloidal sol, this
The surface reinforcing agent that bright technical scheme uses can also be aurosol or gold silver rubber alloy, preferably nanometer silver molten
Glue.
It addition, in above-described embodiment one to four, the laser used is by the laser light of Raman spectrometer self
Source provides, and the laser needed for technical scheme can also be provided by additional LASER Light Source.
It addition, in above-described embodiment one to four, use Matlab7.6 software that dynamic optical spectrogram is carried out pre-place
Obtain the pretreatment Raman spectrogram of blood-sugar lowering tcm drug to be checked after reason, use 2Dshiger version1.3 Software on Drawing
Obtaining the two-dimensional correlation surface-enhanced Raman synchronizable optical spectrogram of blood-sugar lowering tcm drug, the spectrogram used only processes software
It is the basic explanation of technical scheme, it is also possible to select other can one-dimensional Raman spectrogram be carried out
Process the software obtaining two dimension Raman spectrogram.
It addition, the technical scheme that used of embodiment one can also be mixed containing only a kind of alloy or do not contain
The blood-sugar lowering tcm drug to be checked of foreign material is identified, when the two-dimensional correlation surface enhanced raman spectroscopy of blood-sugar lowering tcm drug to be checked
In figure, the peak position that goes out containing the relevant peaks with pioglitazone standard substance differs-w～the relevant peaks of w wave number, then treat
Containing pioglitazone in inspection blood-sugar lowering tcm drug, when the two-dimensional correlation surface enhanced raman spectroscopy figure of blood-sugar lowering tcm drug to be checked
In differ-w～the relevant peaks of w wave number containing the peak position that goes out with the relevant peaks of rosiglitazone standard substance, the most to be checked
Containing rosiglitazone in blood-sugar lowering tcm drug, when in the two-dimensional correlation surface enhanced raman spectroscopy figure of blood-sugar lowering tcm drug to be checked
The peak position that goes out not containing the relevant peaks with pioglitazone and rosiglitazone differs-w～the relevant peaks of w wave number, then
Blood-sugar lowering tcm drug to be checked does not contains pioglitazone and rosiglitazone.
It addition, the technical scheme that above-described embodiment two to four is used, it is also possible to doped with rosiglitazone and
The blood-sugar lowering tcm drug to be checked of two kinds of adulterants of pioglitazone is identified.
It addition, in the technical scheme that above-described embodiment two to four is used, pioglitazone or rosiglitazone phase
Corresponding Rf value is 0.9, and pioglitazone or rosiglitazone involved by technical scheme are corresponding
Can there is certain error in Rf value, between 0.85-0.95.
Claims (7)
1. identifying the method whether adding pioglitazone or rosiglitazone in blood-sugar lowering tcm drug, the method includes: take
Blood-sugar lowering tcm drug to be checked carries out thin layer chromatography, finds doubtful at the Rf value that pioglitazone is corresponding with rosiglitazone
Speckle, it is characterised in that also include three below step:
Step one: the collection of dynamic optical spectrogram
Take surface reinforcing agent point on described doubtful speckle, use Raman spectrometer, choose swashing of some strength
Light carries out perturbation to described doubtful speckle prolonged exposure, and gathers a series of dimensional table of described doubtful speckle
Face strengthens Raman spectrum, obtains the dynamic spectrum of described blood-sugar lowering tcm drug to be checked, every one-dimensional surface-enhanced Raman
The time of integration of spectrum is identical, and described some strength is any number between 100mW～200mW, described
Surface reinforcing agent is aurosol, silver sol or gold silver rubber alloy, and the point sample amount of described surface reinforcing agent is 2 μ L
～10 μ L；
Step 2: the drafting of two-dimensional correlation surface enhanced raman spectroscopy figure
Described dynamic optical spectrogram is carried out pretreatment, including choosing 300cm-1～1700cm-1Spectral coverage, employing
Sgolay method carries out smooth and uses airPLS method to carry out baseline correction, obtains the pre-of described blood-sugar lowering tcm drug to be checked
Process Raman spectrogram, according to described pretreatment Raman spectrogram, draw and obtain described blood-sugar lowering tcm drug to be checked
Two-dimensional correlation surface enhanced raman spectroscopy figure；
Step 3: interpolation pioglitazone or rosiglitazone are identified
According to the described two-dimensional correlation surface enhanced raman spectroscopy figure of described blood-sugar lowering tcm drug to be checked, when in this spectrogram
Differ-w～the relevant peaks of w wave number containing the peak position that goes out with the relevant peaks of described pioglitazone, then judge described
Containing described pioglitazone in blood-sugar lowering tcm drug to be checked, when this spectrogram contains the relevant peaks with described rosiglitazone
Go out peak position difference-w～the relevant peaks of w wave number, then judge in described blood-sugar lowering tcm drug to be checked containing described Roger
Row ketone, when this spectrogram does not contains with described pioglitazone and described rosiglitazone relevant peaks go out peak position
Put difference-w～the relevant peaks of w wave number, then judge described blood-sugar lowering tcm drug to be checked does not contains described pioglitazone and
Described rosiglitazone, w is 1cm-1～5cm-1Between any number, going out of the relevant peaks of described pioglitazone
Peak position is set to: 414cm-1,430cm-1,475cm-1,824cm-1, the relevant peaks of described rosiglitazone go out peak position
For: 739cm-1,1255cm-1,1329cm-1。
Whether qualification blood-sugar lowering tcm drug the most according to claim 1 adds the side of pioglitazone or rosiglitazone
Method, it is characterised in that: described some strength is 200mW.
Whether qualification blood-sugar lowering tcm drug the most according to claim 1 adds the side of pioglitazone or rosiglitazone
Method, it is characterised in that: described two-dimensional correlation surface enhanced raman spectroscopy figure is to synchronize spectrum.
Whether qualification blood-sugar lowering tcm drug the most according to claim 1 adds the side of pioglitazone or rosiglitazone
Method, it is characterised in that: described laser is provided by the LASER Light Source of Raman spectrometer self.
Whether qualification blood-sugar lowering tcm drug the most according to claim 1 adds the side of pioglitazone or rosiglitazone
Method, it is characterised in that: described surface reinforcing agent is nano silver colloidal sol.
Whether qualification blood-sugar lowering tcm drug the most according to claim 1 adds the side of pioglitazone or rosiglitazone
Method, it is characterised in that: the point sample amount of described surface reinforcing agent is 4 μ L～6 μ L.
Whether qualification blood-sugar lowering tcm drug the most according to claim 1 adds the side of pioglitazone or rosiglitazone
Method, it is characterised in that: w is 5cm-1。
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| CN104833669B (en) * | 2015-04-29 | 2018-02-13 | 中国人民解放军第二军医大学 | A kind of quick determination method of weak main ingredient signal medicine |
| CN105223182A (en) * | 2015-09-01 | 2016-01-06 | 中国人民解放军第二军医大学 | A kind of method detecting doped chemical drugs in Chinese patent drug |
| CN105241861B (en) * | 2015-09-18 | 2018-05-08 | 中国人民解放军第二军医大学 | It is a kind of quickly to detect ten kinds of methods for mixing pseudo- component in lipid-loweringing class Chinese patent drug at the same time |
| CN105158194A (en) * | 2015-09-23 | 2015-12-16 | 中国人民解放军第二军医大学 | Method for identifying whether ephedrine and/or pseudo ephedrine are/is added to weight-reducing type traditional Chinese medicine or health care products |
| CN106525809B (en) * | 2016-09-30 | 2019-06-21 | 中国人民解放军第二军医大学 | A method of identifying one of theophylline caffeine theobromine or a variety of chemicals whether are added in relieving cough and asthma class Chinese medicine |
| CN107525859B (en) * | 2017-07-26 | 2020-04-10 | 中国人民解放军第二军医大学 | Method for screening rapid detection conditions of illegally added compound derivatives in health care products |
| CN108732292B (en) * | 2018-04-27 | 2020-07-14 | 中国人民解放军第二军医大学 | Method and device for rapidly detecting sufentanil in blood plasma |
| CN111208112A (en) * | 2020-01-14 | 2020-05-29 | 山西省食品药品检验所(山西省药品包装材料监测中心) | Qualitative detection method for pioglitazone and rosiglitazone in food and medicine |
| CN112986212B (en) * | 2021-03-10 | 2023-01-17 | 中国人民解放军海军军医大学 | Research method for interaction of G-quadruplex aptamer and small molecule |
| CN112986216B (en) * | 2021-05-06 | 2021-07-30 | 江西省药品检验检测研究院 | Method for detecting typical chemical components of skin-care traditional Chinese medicine product by surface enhanced Raman spectroscopy |
| CN113340870A (en) * | 2021-06-09 | 2021-09-03 | 河北省食品检验研究院 | Rapid detection method for illegally added pioglitazone in health food |
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