CN101487827A - Indirect test method for Miglitol purity - Google Patents
Indirect test method for Miglitol purity Download PDFInfo
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- CN101487827A CN101487827A CNA2009100961915A CN200910096191A CN101487827A CN 101487827 A CN101487827 A CN 101487827A CN A2009100961915 A CNA2009100961915 A CN A2009100961915A CN 200910096191 A CN200910096191 A CN 200910096191A CN 101487827 A CN101487827 A CN 101487827A
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- miglitol
- purity
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- methyl
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- 229960001110 miglitol Drugs 0.000 title claims abstract description 82
- IBAQFPQHRJAVAV-ULAWRXDQSA-N Miglitol Chemical compound OCCN1C[C@H](O)[C@@H](O)[C@H](O)[C@H]1CO IBAQFPQHRJAVAV-ULAWRXDQSA-N 0.000 title claims abstract description 81
- 238000010998 test method Methods 0.000 title description 2
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000012360 testing method Methods 0.000 claims abstract description 33
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000005886 esterification reaction Methods 0.000 claims abstract description 27
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000004817 gas chromatography Methods 0.000 claims abstract description 11
- 238000006640 acetylation reaction Methods 0.000 claims abstract description 6
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 6
- 238000010606 normalization Methods 0.000 claims abstract description 6
- 239000000758 substrate Substances 0.000 claims abstract description 6
- 230000021736 acetylation Effects 0.000 claims abstract description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 35
- 239000001301 oxygen Substances 0.000 claims description 35
- 229910052760 oxygen Inorganic materials 0.000 claims description 35
- 230000032050 esterification Effects 0.000 claims description 24
- 239000007788 liquid Substances 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 239000000470 constituent Substances 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 12
- 125000004494 ethyl ester group Chemical group 0.000 claims description 11
- 230000035484 reaction time Effects 0.000 claims description 10
- 238000004587 chromatography analysis Methods 0.000 claims description 6
- 230000014759 maintenance of location Effects 0.000 claims description 4
- 238000005917 acylation reaction Methods 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 claims description 2
- 239000012295 chemical reaction liquid Substances 0.000 abstract 3
- 229960003328 benzoyl peroxide Drugs 0.000 abstract 2
- 238000006555 catalytic reaction Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 10
- 239000000203 mixture Substances 0.000 description 7
- 239000007787 solid Substances 0.000 description 6
- -1 Miglitol ester Chemical class 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 150000008065 acid anhydrides Chemical class 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- 238000005160 1H NMR spectroscopy Methods 0.000 description 2
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N DMSO Substances CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- 230000003292 diminished effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 235000019260 propionic acid Nutrition 0.000 description 2
- 238000012113 quantitative test Methods 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- XVMSFILGAMDHEY-UHFFFAOYSA-N 6-(4-aminophenyl)sulfonylpyridin-3-amine Chemical compound C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=N1 XVMSFILGAMDHEY-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000001212 derivatisation Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 238000003822 preparative gas chromatography Methods 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 238000012956 testing procedure Methods 0.000 description 1
- 208000001072 type 2 diabetes mellitus Diseases 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
- Hydrogenated Pyridines (AREA)
Abstract
The invention discloses an indirect testing method of the purity quotient of miglitol, comprising the following steps: 1) the miglitol to be tested is taken as substrate, and acetic anhydride is taken as acetylation reagent to have acetylation reaction, so that esterification reaction liquid containing acetic acid-beta-(3, 4, 5-triacetyl oxygroup-2-acetoxyl methyl-1-piperidine)-ethyl ester is obtained; or the miglitol to be tested is taken as substrate, propionic andydride is taken as acetylation reagent, and acetylation reaction is carried out under the catalysis of anhydrous pyridine, so that the esterification reaction liquid containing the acetic acid-beta-(3, 4, 5-triacetyl oxygroup-2-acetoxyl methyl-1-piperidine)-ethyl ester is obtained; 2) gas chromatography is carried out on the esterification reaction liquid, and the retaining time and the peak area of all the components in gas chromatograph can be obtained; after the peak area of the light components is eliminated, the purity quotient of the obtained miglitol is calculated according to normalization method. The indirect testing method has the characteristics of simple testing method and accurate testing result.
Description
Technical field
The present invention relates to a kind of indirectly testing method of Miglitol purity.
Background technology
Miglitol is that a kind of type ii diabetes suppresses medicine, and its structure is (I):
Because Miglitol is a polyol, intermolecular force strong (being mainly hydrogen bond), molecular weight is bigger simultaneously, and volatile grade is low, and polarity is strong, can not directly carry out gas chromatography (GC) and detect.At present about the detection multipurpose efficient liquid phase chromatography (HPLC) of Miglitol, there is following weak point: (1) Miglitol is fastidious to detecting device, because of no uv absorption, so can not be with highly sensitive UV-detector; (2) now generally use the parallax refraction detector, but exist the shortcoming that sensitivity is low, be subject to environment temperature and moving phase influence, cause the testing result error big; (3) this method is to the equipment requirements height, and complicated operation.
Compare with HPLC, GC has fast, highly sensitive and easy and simple to handle, the widely used advantage of detection speed, if the purity that therefore can utilize GC to obtain Miglitol indirectly just is necessary very much.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of indirectly testing method of Miglitol purity.
In order to solve the problems of the technologies described above, the invention provides a kind of indirectly testing method of Miglitol purity, may further comprise the steps:
1), with Miglitol to be measured as substrate, aceticanhydride carries out acetylization reaction as acetylation reagent, aceticanhydride: the mass ratio of Miglitol=3～30:1,85～105 ℃ of temperature of reaction, reaction time 1～3h; The esterification liquid that must contain acetate-β-(3,4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-ethyl ester;
2), to containing acetate-β-(3,4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-the esterification liquid of ethyl ester carries out gas chromatographic analysis, obtain retention time and the peak area of its each component in gas chromatography, after removing the peak area of light constituent, calculate the purity that obtains Miglitol according to normalization method.
As the improvement of the indirectly testing method of Miglitol purity of the present invention, aceticanhydride: the mass ratio of Miglitol=10～13:1,90～100 ℃ of temperature of reaction, reaction time 2h.
Another kind as the indirectly testing method of Miglitol purity of the present invention improves, and step 1) adopts anhydrous pyridine as catalyzer, anhydrous pyridine: the mass ratio of Miglitol=0.4～0.8:1, reaction time 1～2.5h.
As the further improvement of the indirectly testing method of Miglitol purity of the present invention, aceticanhydride: the mass ratio of Miglitol=7～10:1,90～100 ℃ of temperature of reaction, reaction time 2h.
The present invention also provides the indirectly testing method of another kind of Miglitol purity simultaneously, may further comprise the steps:
1), with Miglitol to be measured as substrate, propionic andydride is as acylating reagent, under the catalytic action of anhydrous pyridine, carry out acylation reaction, propionic andydride: the mass ratio of Miglitol=8～12:1, anhydrous pyridine: the mass ratio of Miglitol=0.4～0.8:1,95～100 ℃ of temperature of reaction, reaction time 2～2.5h; The esterification liquid that must contain propionic acid-β-(3,4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-ethyl ester;
2), to propionic acid-β-(3,4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-the esterification liquid of ethyl ester carries out gas chromatographic analysis, obtain retention time and the peak area of its each component in gas chromatography, after removing the peak area of light constituent, calculate the purity that obtains Miglitol according to normalization method.
The step 1) of the inventive method can be shown below:
Wherein
The indirectly testing method of Miglitol purity of the present invention owing at first the Miglitol esterification is derived, thereby has been eliminated the hydrogen bond action of molecular link, therefore can significantly improve its volatile grade, so that carry out quantitative test (gas chromatographic detection).Testing procedure can be undertaken by following scheme: get esterification liquid and detect as the direct air inlet chromatography of sample, carry out normalization after removing the peak of carboxylic acid, acid anhydrides and these light components of pyridine in the spectrogram that obtains, can learn the purity of Miglitol.
In sum, the indirectly testing method of Miglitol purity of the present invention, utilize the gas chromatographic detection method to carry out quantitative test, utilize derivatization method effectively to improve the Miglitol volatile grade and the character that in GC, is detected, solved the problem that Miglitol can not adopt the GC method to detect.
The indirectly testing method of Miglitol purity of the present invention, its characteristics are: with low-cost, highly sensitive vapor-phase chromatography, substituted the liquid chromatography of original expensive, muting sensitivity parallax refraction detector.Therefore, the present invention has simple, the accurate test result characteristics of method of testing.
The present invention [is promptly contained acetate-β-(3 at the full esterification derivative of Miglitol of step 1) gained, 4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-the esterification liquid of ethyl ester or contain propionic acid-β-(3,4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-and the esterification liquid of ethyl ester] extract, can obtain light grey pulverous acetate-β-(3,4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-ethyl ester [or propionic acid-β-(3,4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-ethyl ester].Extracting method is: the decompression of esterification liquid is taken off light constituent (carboxylic acid of generation, intact acid anhydrides, the intact catalyzer anhydrous pyridine of unreacted of unreacted) to syrupy shape, add 2～5 times of volume deionized waters, leave standstill 1～2h under the room temperature and separate out solid, filtration under diminished pressure, washing, 50 ℃ of oven dry of solid.
Description of drawings
Below in conjunction with accompanying drawing the specific embodiment of the present invention is described in further detail.
Fig. 1 is acetate-β of the present invention-H-NMR of (3,4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-ethyl ester (being pentaacetic acid Miglitol ester) and the atom numbering figure that is wherein adopted.
Fig. 2 is propionic acid-β of the present invention-H-NMR of (3,4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-ethyl ester (i.e. five propionic acid Miglitol esters) and the atom numbering figure that is wherein adopted.
Embodiment
The indirectly testing method of embodiment 1, a kind of Miglitol purity may further comprise the steps:
1), adds 1.86g Miglitol white powder to be measured (being pure product) in the 50ml there-necked flask, the 17ml aceticanhydride, the 1ml anhydrous pyridine, mechanical raking, air set pipe refluxes, 93～97 ℃ of control heating-up temperatures, stop reaction behind the reaction 2h, the esterification liquid that must contain acetate-β-(3,4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-ethyl ester (is approximately 20～25ml).
2), direct sample detects to above-mentioned esterification liquid, supporting hydrogen flame monitor of used gas chromatograph and temperature programme, obtain containing acetate-β-(3,4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-ethyl ester, light constituent (the acetate of generation, the aceticanhydride that unreacted is intact, the catalyzer anhydrous pyridine that unreacted is intact) gas chromatogram, after removing light constituent peak area is carried out normalized, thereby learn acetate-β-(3,4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-ethyl ester quality percentage composition is 99.9%, does not have other impurity.Because Miglitol all has been transformed into acetate-β-(3,4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-ethyl ester, calculates to such an extent that Miglitol purity is 99.9%.
Projectional technique is as follows:
With acetate-β-(3,4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-the quality percentage composition of ethyl ester is scaled molar content, this molar content is consistent with the molar content of Miglitol in the testing sample, obtained molar content, again it is scaled the quality percentage composition, is sample Miglitol purity.
Miglitol sample actual purity to be measured is 100%, and test accuracy is 99.9%.
The esterification liquid that contains acetate-β-(3,4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-ethyl ester that obtains with the described method of the step 1) of embodiment 1 is fully extracted, and extracting method is as follows:
Light constituent (acetate of generation, intact acid anhydrides, the intact catalyzer anhydrous pyridine of unreacted of unreacted) is taken off in this esterification liquid decompression, add the deionized water of 2～5 times of volumes, leave standstill 1～2h under the room temperature to syrupy shape, separate out solid, filtration under diminished pressure, washing, 50 ℃ of oven dry of solid.The gained solid detects through HNMR, proves that its structure is acetate-β-(3,4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-ethyl ester, and HNMR collection of illustrative plates and atom numbering thereof are schemed as shown in Figure 1, among Fig. 1:
HNMR(400MHz，d
6-DMSO)：4.99～5.04(t，1H，4-H)，4.83～4.88(t，1H，5-H)，4.75～4.81(m，1H，3-H)，4.03～4.17(m，4H，8-2H，21-2H)，3.09～3.13(t，1H，6-H)，2.83～3.00(m，3H，2-H，7-2H)，2.58～2.64(t，1H，2-H)，2.01(s，3H，CH
3)，2.00(s，3H，CH
3)，1.99(s，3H，CH
3)，1.98(s，3H，CH
3)，1.96(s，3H，CH
3)
Structural formula is suc as formula 1:
(formula 1)
The indirectly testing method of embodiment 2, a kind of Miglitol purity may further comprise the steps:
1), adds 1.86g Miglitol white powder (forming) to be measured in the 50ml there-necked flask by the pure product Miglitol of 1.60g+0.26g sorbierite, the 20ml aceticanhydride, mechanical raking, air set pipe refluxes, 93～97 ℃ of control heating-up temperatures, reaction 2h, stop reaction, the esterification liquid that must contain acetate-β-(3,4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-ethyl ester (structural formula is suc as formula 1).
2), direct sample detects to above-mentioned esterification liquid, supporting hydrogen flame monitor of used gas chromatograph and temperature programme, obtain containing acetate-β-(3,4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-gas chromatogram of ethyl ester and impurity (sorbierite esterification thing), light constituent (acetate, the intact aceticanhydride of unreacted that comprise generation).After removing light constituent peak area is carried out normalized, draw acetate-β-(3,4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-ethyl ester quality percentage composition is 84.7%, because Miglitol all has been transformed into acetate-β-(3,4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-ethyl ester, calculate to such an extent that Miglitol purity is 86.7%.
Miglitol sample actual purity to be measured is 86.0%, and test accuracy is 99.2%.
The indirectly testing method of embodiment 3, a kind of Miglitol purity, the Miglitol white powder that the 1.86g among the embodiment 2 is to be measured make into to be made up of the pure product Miglitol of 1.50g+0.36g sorbierite, and all the other contents are with embodiment 2; The gained result is as follows:
Acetate-β-(3,4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-ethyl ester quality percentage composition is 78.6%, because Miglitol all has been transformed into acetate-β-(3,4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-ethyl ester, calculate to such an extent that Miglitol purity is 81.2%.
Miglitol sample actual purity to be measured is 80.6%, and test accuracy is 99.3%.
The indirectly testing method of embodiment 4, a kind of Miglitol purity, carry out following steps successively:
1), adds 2.17g Miglitol white powder (being pure product) in the 50ml there-necked flask, the 22ml propionic andydride, the 1ml anhydrous pyridine, mechanical raking, air set pipe refluxes, 93～97 ℃ of control heating-up temperatures, reaction 2.5h stops reaction, must contain propionic acid-β-(3,4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-the esterification liquid of ethyl ester.
2), direct sample detects to above-mentioned esterification liquid, supporting hydrogen flame monitor of used gas chromatograph and temperature programme, obtain containing propionic acid-β-(3,4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-gas chromatogram of ethyl ester, light constituent (propionic acid of generation, intact propionic andydride, the intact catalyzer anhydrous pyridine of unreacted of unreacted), after removing light constituent peak area is carried out normalized, thereby learn propionic acid-β-(3,4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-ethyl ester quality percentage composition is 99.9%.Because Miglitol all has been transformed into propionic acid-β-(3,4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-ethyl ester, calculates to such an extent that Miglitol purity is 99.9%.
Miglitol sample actual purity to be measured is 100%, and test accuracy is 99.9%.
Equally, to fully contain propionic acid-β-(3 with what the described method of the step 1) of embodiment 4 obtained, 4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-and the esterification liquid of ethyl ester carries out extracting method, and extracting method is the same, the gained solid detects through HNMR, prove that its structure is propionic acid-β-(3,4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-ethyl ester, its HNMR spectrogram and atom numbering are schemed as shown in Figure 2, among Fig. 2:
HNMR(400MHz，d
6-DMSO)：5.14～5.16(t，1H，4-H)，4.51～4.59(m，2H，3-H，5-H)，4.16～4.28(m，3H，8-2H，21-H)，3.99～4.02(d，1H，21-H)，3.40～3.43(m，1H，6-H)，2.58～2.66(m，3H，2-H，7-2H)，2.33～2.39(t，1H，2-H)，2.25～2.31(q，10H，5CH
2)，1.10～1.17(t，15H，5CH
3)
Structural formula is as shown in Equation 2:
(formula 2)
The indirectly testing method of embodiment 5, a kind of Miglitol purity, the Miglitol that the 2.17g among the embodiment 4 is to be measured make into to be made up of the pure product Miglitol of 1.91g+0.26g sorbierite, and all the other contents are with embodiment 4; The gained result is as follows:
Propionic acid-β-(3,4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-ethyl ester amount percentage composition is 86.3%, because Miglitol all has been transformed into acetate-β-(3,4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-ethyl ester, calculate to such an extent that Miglitol purity is 88.4%.
Miglitol sample actual purity to be measured is 88.0%, and test accuracy is 99.5%.
At last, it is also to be noted that what more than enumerate only is several specific embodiments of the present invention.Obviously, the invention is not restricted to above embodiment, many distortion can also be arranged.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.
Claims (5)
1, a kind of indirectly testing method of Miglitol purity is characterized in that may further comprise the steps:
1), with Miglitol to be measured as substrate, aceticanhydride carries out acetylization reaction as acetylation reagent, aceticanhydride: the mass ratio of Miglitol=3～30:1,85～105 ℃ of temperature of reaction, reaction time 1～3h; The esterification liquid that must contain acetate-β-(3,4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-ethyl ester;
2), to containing acetate-β-(3,4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-the esterification liquid of ethyl ester carries out gas chromatographic analysis, obtain retention time and the peak area of its each component in gas chromatography, after removing the peak area of light constituent, calculate the purity that obtains Miglitol according to normalization method.
2, the indirectly testing method of Miglitol purity according to claim 1 is characterized in that: aceticanhydride: the mass ratio of Miglitol=10～13:1,90～100 ℃ of temperature of reaction, reaction time 2h.
3, the indirectly testing method of Miglitol purity according to claim 1 is characterized in that: described step 1) adopts anhydrous pyridine as catalyzer, anhydrous pyridine: the mass ratio of Miglitol=0.4～0.8:1, reaction time 1～2.5h.
4, the indirectly testing method of Miglitol purity according to claim 3 is characterized in that: aceticanhydride: the mass ratio of Miglitol=7～10:1,90～100 ℃ of temperature of reaction, reaction time 2h.
5, a kind of indirectly testing method of Miglitol purity is characterized in that may further comprise the steps:
1), with Miglitol to be measured as substrate, propionic andydride is as acylating reagent, under the catalytic action of anhydrous pyridine, carry out acylation reaction, propionic andydride: the mass ratio of Miglitol=8～12:1, anhydrous pyridine: the mass ratio of Miglitol=0.4～0.8:1,95～100 ℃ of temperature of reaction, reaction time 2～2.5h; The esterification liquid that must contain propionic acid-β-(3,4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-ethyl ester;
2), to propionic acid-β-(3,4,5-triacetyl oxygen base-2-acetyl-o-methyl-1-piperidines)-the esterification liquid of ethyl ester carries out gas chromatographic analysis, obtain retention time and the peak area of its each component in gas chromatography, after removing the peak area of light constituent, calculate the purity that obtains Miglitol according to normalization method.
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