CN101504379A - Medicinal smectite X-ray diffraction map identification standard - Google Patents
Medicinal smectite X-ray diffraction map identification standard Download PDFInfo
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Abstract
The invention discloses an identification standard for an X-ray diffraction pattern of pharmaceutical montmorillonite, which is characterized in that characteristic spectral lines of the X-ray diffraction pattern of montmorillonite are positioned at wavelengths of about 1.5nm and about 0.45nm, and intensities of other impurity peaks in the pattern cannot be higher than a second characteristic peak (at about 0.45nm wavelength) of the montmorillonite, wherein the sum of the intensities of two impurity peaks at wavelengths of about 0.40nm and about 0.3nm cannot be higher than the second characteristic peak (at about 0.45nm wavelength) of the montmorillonite.
Description
Invention field
The present invention relates to a kind of medicinal smectite X-ray diffraction map identification standard, belong to drug standards technical field.
Background technology
Smectite is through the proof of clinical practice for many years treatment diarrhoeal diseases determined curative effect, the medicine that toxic and side effect is little.
Smectite is bentonitic principal ingredient.Because the bentonitic minerogentic condition in various places differs, wherein the mineral of the content of smectite and association thereof are also different, are exactly same ore deposit point, and its smectite content of different ore beds also has than big difference.Mineral normal and the smectite association have illite, quartz, secondary quartz, feldspar, kalzit, rauhkalk etc.That smectite has is water insoluble, water-swellable, become the characteristic of colloidal solution in water.The natural particle diameter of smectite is minimum, mainly be present in＜scope of 2 μ m in, thereby surface energy is bigger, generally all be gathered into bigger particle, and the particle diameter of other composition is distributed in mainly the scope of 10 μ m.Use the above-mentioned characteristic of smectite, according to Stokes formula, spheroid square being directly proportional of decline rate and its radius in solution is so the mineral of smectite and association have settling velocity than big difference in water.Utilize this principle, get bentonitic clay and add aqueous dispersion, just can obtain highly purified medicinal smectite with sedimentation or rotational flow separation method.
Smectite has its own specific X ray diffracting spectrum, and distance between diffraction maximum and relative intensity thereof can be used as the discriminating or the quantitative test of smectite.One of discrimination method of existing medicinal smectite quality standard, differentiate with X ray diffracting spectrum, method is: it is an amount of to get smectite, when putting 20 ℃ in the exsiccator of relative humidity 75%, placed about 12 hours, measure the record collection of illustrative plates according to x-ray powder diffraction (Chinese Pharmacopoeia version appendix in 2005 IX F).The characteristic spectral line of smectite is at about 1.5nm and 0.45nm wavelength place, and other impurity peaks intensity must not be higher than second characteristic peak (about 0.45nm wavelength place) of smectite in the collection of illustrative plates.
There is major defect in the X ray diffracting spectrum judging standard of existing medicinal smectite quality standard, because the bentonitic minerogentic condition in the different places of production differs, wherein the mineral of the content of smectite and association thereof are also different, be exactly same ore deposit point, the mineral species of its smectite content of different ore beds and association also has than big difference.Existing medicinal smectite quality standard is differentiated in the item and has only been stipulated that " other impurity peaks intensity must not be higher than second characteristic peak (about 0.45nm wavelength place) of smectite in the collection of illustrative plates." this regulation is in order to limit the content of smectite impurities; smectite contains two or more impurity; though the impurity peaks intensity in the X ray diffracting spectrum is not higher than second characteristic peak of smectite; if but intensity is bigger; and its intensity sum is greater than second characteristic peak of smectite; then the amount of smectite impurities also is many, but still meet existing medicinal smectite X-ray diffraction map identification standard, although it is qualified to detect with existing medicinal smectite quality standard, smectite content is still lower in fact, thereby influences the quality and the curative effect of medicine.
We find that in test the X ray diffracting spectrum impurity peaks intensity of the medicinal smectite raw material of the manufacturer production that has and smectite preparation is less, and the X ray diffracting spectrum impurity peaks intensity of the medicinal smectite raw material of the manufacturer production that has and smectite preparation is bigger.Major impurity peak spectral line is at about 0.40nm wavelength place and about 0.33nm wavelength place.All qualified with existing medicinal smectite quality standard check, as seen the X ray diffracting spectrum judging standard of existing medicinal smectite quality standard can not be controlled the medicinal smectite quality effectively, and impurity is more, can not guarantee clinical efficacy.
We are to medicinal smectite standard items, medicinal smectite raw material and preparation thereof, measure X ray diffracting spectrum, and to adsorb the amount calculating smectite content of methylene blue, found that: impurity peaks intensity sum becomes negative correlation with the content of smectite in the X ray diffracting spectrum, impurity peaks intensity sum is big, and the content of smectite is low.
By the X ray diffracting spectrum judging standard of existing medicinal smectite quality standard, the producer can get the bentonitic clay in the different places of production, mixes in the constant weight ratio, converts the smectite that becomes to meet existing medicinal smectite quality standard.Also can get the bentonitic clay in the different places of production, wash refining not according to the technology strict demand, get medicinal smectite without sedimentation or rotational flow separation legal system, but the bentonitic clay of getting the different places of production is simply washed, mix in the constant weight ratio, convert the smectite that becomes to meet existing medicinal smectite quality standard, and X ray diffracting spectrum is also up to specification.
We also send out in test the bentonitic clay X ray diffracting spectrum existing, and except that the characteristic spectral line of smectite, other major impurity peak is at about 0.40nm wavelength place in the collection of illustrative plates.The bentonitic clay X ray diffracting spectrum that has, except that the characteristic spectral line of smectite, other major impurity peak is at about 0.33nm wavelength place in the collection of illustrative plates.If the bentonitic clay with the single place of production prepares medicinal smectite, after must fully stirring with a large amount of water, to place, natural subsidence was got the top suspension more than 24 hours, discarded the dirt of association, removed moisture, drying.Or after fully stirring with a large amount of water, repeatedly use the rotational flow separation method, and remove the dirt of association, just can make the smectite that X ray diffracting spectrum meets medicinal standard.If with X ray diffracting spectrum major impurity peak at the bentonitic clay of about 0.40nm and X ray diffracting spectrum major impurity peak the bentonitic clay at about 0.33nm wavelength, mix by certain weight ratio, adding water stirs, cross 325 mesh sieves and remove the sandstone of bulk, drying and crushing, without sedimentation or rotational flow separation method repeatedly, can obtain meeting the smectite of existing medicinal smectite quality standard equally, and X ray diffracting spectrum meets the X ray diffracting spectrum standard of existing medicinal smectite quality standard.
Often contain water-soluble salt in the bentonitic clay raw ore, the simple washing of bentonitic clay warp desalination with the different places of production, sieve and remove the sandstone of bulk, press the certain weight ratio mixing, can obtain meeting the smectite of existing medicinal smectite quality standard, and X ray diffracting spectrum also meets the X ray diffracting spectrum standard of existing medicinal smectite quality standard.
This smectite that obtains with mixing method, although smectite content is low, but still meet the diagnostic characteristics of the X ray diffracting spectrum of existing medicinal smectite quality standard, promptly at the characteristic spectral line of the apparent smectite of about 1.5nm and 0.45nm wavelength place, other impurity peaks intensity is not higher than second characteristic peak (about 0.45nm wavelength place) of smectite in the collection of illustrative plates.This smectite that obtains with mixing method, the major impurity peak spectral line of X ray collection of illustrative plates is at about 0.40nm wavelength place and about 0.33nm wavelength place, peak intensity all is not higher than second characteristic peak (about 0.45nm wavelength place) of smectite, but two impurity peaks intensity sums at about 0.40nm wavelength place and about 0.33nm wavelength place are higher than second characteristic peak (about 0.45nm wavelength place) of smectite.
We buy commercially available medicinal smectite and preparation thereof, be up to the standards by existing medicinal smectite quality standard, but the major impurity peak of repeatedly finding its X ray collection of illustrative plates is at about 0.40nm wavelength place and about 0.33nm wavelength place, intensity all is not higher than second characteristic peak (about 0.45nm wavelength place) of smectite, but the peak intensity sum at about 0.40nm wavelength place and about 0.33nm wavelength place is higher than second characteristic peak (about 0.45nm wavelength place) of smectite, is to get with the bentonitic clay in the different places of production is mixed through verifying through investigation.
As seen the X ray diffracting spectrum judging standard of existing medicinal smectite quality standard can not be controlled the medicinal smectite quality effectively, and the smectite that content is lower also can meet medicinal standard, and then can influence clinical efficacy.
The objective of the invention is, the defective for the X ray diffracting spectrum judging standard that overcomes existing medicinal smectite quality standard exists provides a kind of X ray diffracting spectrum judging standard that can control the medicinal smectite quality effectively.
Summary of the invention
The invention discloses a kind of X ray diffracting spectrum judging standard of medicinal smectite.
The X ray diffracting spectrum judging standard of a kind of medicinal smectite of the present invention is: the characteristic spectral line of smectite X-ray diffraction map is at about 1.5nm and about 0.45nm wavelength place, other impurity peaks intensity must not be higher than second characteristic peak (about 0.45nm wavelength place) of smectite in the collection of illustrative plates, and wherein two impurity peaks intensity sums at about 0.40nm wavelength place and about 0.33nm wavelength place must not be higher than second characteristic peak (about 0.45nm wavelength place) of smectite.
The X ray diffracting spectrum judging standard of a kind of medicinal smectite of the present invention, the X ray diffracting spectrum assay method is: get smectite an amount of (about 3g), when putting 20 ℃ in the exsiccator of relative humidity 75%, placed about 12 hours, measure the record collection of illustrative plates according to x-ray powder diffraction (Chinese Pharmacopoeia version appendix in 2005 IX F).
The X ray diffracting spectrum judging standard of a kind of medicinal smectite of the present invention, the X ray diffracting spectrum judging standard that can be used for the smectite preparation, method is: get smectite preparation an amount of (containing smectite 3g approximately), solubilizer, stir, filter, remove auxiliary material, filter cake is after drying below 105 ℃, when putting 20 ℃ in the exsiccator of relative humidity 75%, placed about 12 hours, measure according to x-ray powder diffraction (Chinese Pharmacopoeia version appendix in 2005 IX F), the record collection of illustrative plates, the characteristic spectral line of smectite X-ray diffraction map is at about 1.5nm and about 0.45nm wavelength place, other impurity peaks intensity must not be higher than second characteristic peak (about 0.45nm wavelength place) of smectite in the collection of illustrative plates, and wherein two impurity peaks intensity sums at about 0.40nm wavelength place and about 0.33nm wavelength place must not be higher than second characteristic peak (about 0.45nm wavelength place) of smectite.
Solvent described in the said method comprises the mixed liquor of methyl alcohol, Different concentrations of alcohol and the methyl alcohol of water, Different concentrations of alcohol, variable concentrations.
The X ray diffracting spectrum judging standard of a kind of medicinal smectite of the present invention, the X ray diffracting spectrum judging standard that can be used for the smectite preparation, can also get smectite preparation an amount of (containing smectite 3g approximately), be ground into fine powder, when putting 20 ℃ in the exsiccator of relative humidity 75%, placed about 12 hours, and measured, the record collection of illustrative plates according to x-ray powder diffraction (Chinese Pharmacopoeia version appendix in 2005 IX F).The characteristic spectral line of smectite X-ray diffraction map is at about 1.5nm and about 0.45nm wavelength place, in the collection of illustrative plates except that auxiliary material, other impurity peaks intensity must not be higher than second characteristic peak (about 0.45nm wavelength place) of smectite, and wherein two impurity peaks intensity sums at about 0.40nm wavelength place and about 0.33nm wavelength place must not be higher than second characteristic peak (about 0.45nm wavelength place) of smectite.
Smectite preparation of the present invention comprises clinical formulations commonly used such as powder, tablet, capsule, granule, supensoid agent, gel, dispersing tablet.
The present invention compared with prior art has following advantage: can control the content of medicinal smectite impurity effectively, guarantee the quality of medicinal smectite and preparation thereof, and then guarantee the clinical efficacy of smectite.
The implication of relevant technologies feature of the present invention is explained." characteristic spectral line of smectite is at about 1.5nm and 0.45nm wavelength place ", the X ray diffracting spectrum eigenwert is to identify the main foundation of thing phase, but because the difference of sample and test condition and ennuple state and inevitable measuring error, making between measured value and the mark value of pushing away has a deviation, in the index of " powdery diffractometry card group " that the international powdery diffractometry standard of the bias of permission joint conference edits and publishes regulation is arranged.So the present invention uses " characteristic spectral line of smectite is at about 1.5nm and 0.45nm wavelength place ", this record form is consistent with the X ray diffracting spectrum discrimination method record form of the existing medicinal smectite quality standard that country issues." other impurity peaks intensity must not be higher than second characteristic peak (about 0.45nm wavelength place) of smectite in the collection of illustrative plates ", this record form is consistent with the X ray diffracting spectrum discrimination method record form of the existing medicinal smectite quality standard that country issues, implication is, other impurity peaks intensity must not be higher than second characteristic peak of smectite in the collection of illustrative plates, promptly must not be higher than the characteristic peak of smectite at about 0.45nm wavelength place." get smectite an amount of (about 3g) ", bracket indicates that the literal of note is one of basic usage of bracket in the style of writing, and the implication here is to get about 3g, and relevant precision regulation takes by weighing 3g in the Chinese Pharmacopoeia note on the use, means that the amount of taking by weighing can be 2.5-3.5g.The implication of " measuring according to x-ray powder diffraction (Chinese Pharmacopoeia version appendix in 2005 IX F) " is: according to two appendix IX of Chinese Pharmacopoeia version in 2005 F, the method for the x-ray powder diffraction of record regulation is operated.All be with this form record assay method in Chinese Pharmacopoeia, the ministry of Health of China drug standards and the State Food and Drug Administration's drug standards.X ray diffracting spectrum medium wavelength unit is a dust, and quality standard medium wavelength unit is a nanometer, and the two can convert mutually.
Description of drawings
Accompanying drawing 1 is the X ray diffracting spectrum of medicinal smectite standard items.
Accompanying drawing 2 is major impurity peak bentonitic clays at about 0.40nm wavelength place, after the water that adds 10 times of amounts fully stirs, crosses 325 mesh sieves, removes the sandstone of bulk, centrifugal dewatering, and filter cake is pulverized the X ray diffracting spectrum of back sample in dry below 105 ℃.
Accompanying drawing 3 is major impurity peak bentonitic clays at about 0.33nm wavelength place, after the water that adds 8 times of amounts fully stirs, crosses 325 mesh sieves, removes the sandstone of bulk, centrifugal dewatering, and filter cake is pulverized the X ray diffracting spectrum of back sample in dry below 105 ℃.
Accompanying drawing 5 is with the bentonitic clay of X ray diffracting spectrum major impurity peak at about 0.33nm wavelength place, the X ray diffracting spectrum of the medicinal smectite of preparation.
Embodiment
Embodiment below with reference to the accompanying drawings describes the present invention in detail.
Taking by weighing the smectite standard items (purchases in Chinese pharmaceutical biological product and identifies institute, lot number: 100860-200501) 2.6g, in the exsiccator of relative humidity 75%, placed about 12 hours when putting 20 ℃, measure the record collection of illustrative plates according to x-ray powder diffraction (Chinese Pharmacopoeia version appendix in 2005 IX F).X ray diffracting spectrum shows the characteristic spectral line of smectite at 1.52nm and 0.449nm wavelength place, in the collection of illustrative plates at 0.501nm, 0.407nm, 0.334nm, 0.321nm, 0.258nm the equiwavelength locates to show the impurity peaks spectral line, impurity peaks intensity all is not higher than second characteristic peak (0.449nm wavelength place) of smectite, wherein two impurity peaks intensity at 0.407nm wavelength place and about 0.334nm wavelength place are respectively 20,15, both intensity sums are 35, second characteristic peak (0.449nm) intensity of smectite is 54, in two impurity peaks intensity sums at 0.407nm wavelength place and about 0.334nm wavelength place intensity less than second characteristic peak (0.449nm) of smectite.All other indexs are measured by existing smectite quality standard, all up to specification, conclusion: this smectite had both met the X ray diffracting spectrum judging standard of existing medicinal smectite quality standard, met the X ray diffracting spectrum judging standard of a kind of medicinal smectite of the present invention again.
Get the bentonitic clay of major impurity peak at about 0.40nm wavelength place, after the water that adds 10 times of amounts fully stirs, cross 325 mesh sieves, remove the sandstone of bulk, centrifugal dewatering, filter cake is pulverized in dry below 105 ℃, takes by weighing this product 3g, when putting 20 ℃ in the exsiccator of relative humidity 75%, placed about 12 hours, and measured, the record collection of illustrative plates according to x-ray powder diffraction (Chinese Pharmacopoeia version appendix in 2005 IX F).X ray diffracting spectrum shows the characteristic spectral line of smectite at 1.538nm and 0.449nm wavelength place, locate to show the impurity peaks spectral line 0.504nm, 0.405nm, 0.335nm, 0.303nm, 0.248nm equiwavelength in the collection of illustrative plates, be respectively 40 wherein in 0.405nm wavelength place impurity peaks intensity, second characteristic peak (0.449nm) intensity of smectite is 29, greater than the intensity of second characteristic peak (0.449nm) of smectite.All other indexs are measured by existing smectite quality standard, and are all up to specification, conclusion: judge by existing medicinal smectite quality standard, and defective.
Get the bentonitic clay of major impurity peak at about 0.33nm wavelength place, after the water that adds 8 times of amounts fully stirs, cross 325 mesh sieves, remove the sandstone of bulk, centrifugal dewatering, filter cake is pulverized in dry below 105 ℃, takes by weighing this product 3.3g, when putting 20 ℃ in the exsiccator of relative humidity 75%, placed about 12 hours, and measured, the record collection of illustrative plates according to x-ray powder diffraction (Chinese Pharmacopoeia version appendix in 2005 IX F).X ray diffracting spectrum shows the characteristic spectral line of smectite at 1.512nm and 0.448nm wavelength place, locate to show the impurity peaks spectral line 0.504nm, 0.426nm, 0.334nm, 0.301nm, 0.256nm equiwavelength in the collection of illustrative plates, wherein be 27 in 0.334nm wavelength place impurity peaks intensity, second characteristic peak (0.448nm) intensity of smectite is 19, in the intensity of 0.334nm wavelength place impurity peaks intensity greater than second characteristic peak (0.448nm) of smectite.All other indexs are measured by existing smectite quality standard, and are all up to specification, conclusion: judge by existing medicinal smectite quality standard, and defective.
Get the sample of embodiment 2 and embodiment 3 preparations respectively, mix, take by weighing 3.3g by 1: 1 weight ratio, when putting 20 ℃ in the exsiccator of relative humidity 75%, placed about 12 hours, and measured, the record collection of illustrative plates according to x-ray powder diffraction (Chinese Pharmacopoeia version appendix in 2005 IXF).X ray diffracting spectrum shows the characteristic spectral line of smectite at 1.522nm and 0.450nm wavelength place, in the collection of illustrative plates at 0.502nm, 0.428nm, 0.406nm, 0.335nm, 0.257nm the equiwavelength locates to show the impurity peaks spectral line, impurity peaks intensity all is not higher than second characteristic peak (0.450nm wavelength place) of smectite, wherein two impurity peaks intensity at 0.406nm wavelength place and 0.335nm wavelength place are respectively 19,23, both intensity sums are 42, second characteristic peak (0.450nm) intensity of smectite is 26, in two impurity peaks intensity sums at 0.406nm wavelength place and about 0.335nm wavelength place intensity greater than second characteristic peak (0.450nm) of smectite.All other indexs are measured by existing smectite quality standard, and are all up to specification, conclusion: judge by existing medicinal smectite quality standard, and qualified.The X ray diffracting spectrum judging standard of a kind of medicinal smectite of the present invention is judged, and is defective.
Above-mentioned 4 embodiment, two underproof samples as can be seen, after certain weight ratio mixing, X ray diffracting spectrum judging standard by existing medicinal smectite quality standard is checked, but be qualified, as seen have the defective of the X ray diffracting spectrum judging standard of medicinal smectite quality standard now.
Get the bentonitic clay of major impurity peak, after the water that adds 8 times of amounts fully stirs, placed 24 hours at about 0.33nm wavelength place, draw the top suspension, discard bottom impurity, filter, filter cake is in dry below 105 ℃, pulverize, take by weighing this product 3.3g, in the exsiccator of relative humidity 75%, placed about 12 hours when putting 20 ℃, measure the record collection of illustrative plates according to x-ray powder diffraction (Chinese Pharmacopoeia version appendix in 2005 IX F).X ray diffracting spectrum shows the characteristic spectral line of smectite at 1.471nm and 0.446nm wavelength place, in the collection of illustrative plates at 0.491nm, 0.333nm, 0.299nm, 0.254nm the equiwavelength locates to show the impurity peaks spectral line, impurity peaks intensity all is not higher than second characteristic peak (0.446nm wavelength place) of smectite, wherein at inclusion-free peak, about 0.40nm wavelength place, impurity peaks intensity is 25 at 0.333nm wavelength place, both intensity sums are 25, second characteristic peak (0.446nm) intensity of smectite is 45, in two impurity peaks intensity sums at about 0.40nm and 0.333nm wavelength place intensity less than second characteristic peak (0.446nm) of smectite.All other indexs are measured by existing smectite quality standard, and are all up to specification.Conclusion: judge by existing medicinal smectite quality standard, qualified.X ray diffracting spectrum judging standard by a kind of medicinal smectite of the present invention is judged, and is qualified.
Get the diffusing bag of commercially available smectite, contain smectite 3g, add water 50ml, stir, filter, 3 times repeatedly, remove auxiliary material, after the drying, be ground into fine powder, in the exsiccator of relative humidity 75%, placed about 12 hours when putting 20 ℃, measure the record collection of illustrative plates according to x-ray powder diffraction (Chinese Pharmacopoeia version appendix in 2005 IXF).X ray diffracting spectrum shows the characteristic spectral line of smectite at 1.502nm and 0.448nm wavelength place, locate to show the impurity peaks spectral line 0.401nm, 0.332nm, 0.254nm equiwavelength in the collection of illustrative plates, impurity peaks intensity all is not higher than second characteristic peak (0.446nm wavelength place) of smectite, be respectively that 18,23 both intensity sums are 41 wherein at about 0.401nm wavelength place with in 0.332nm wavelength place impurity peaks intensity, second characteristic peak (0.448nm) intensity of smectite is the intensity of 36, two impurity peaks intensity sums greater than second characteristic peak (0.448nm) of smectite.All other indexs are measured by existing smectite quality standard, and are all up to specification.Conclusion: judge by existing medicinal smectite quality standard, qualified.X ray diffracting spectrum judging standard by a kind of medicinal smectite of the present invention is judged, and is defective.
Get 6 of commercially available smectite dispersing tablets, contain smectite 3g, be ground into fine powder, in the exsiccator of relative humidity 75%, placed about 12 hours when putting 20 ℃, measure, the record collection of illustrative plates according to x-ray powder diffraction (Chinese Pharmacopoeia version appendix in 2005 IXF).X ray diffracting spectrum shows the characteristic spectral line of smectite at 1.514nm and 0.449nm wavelength place, be respectively that 11,16 both intensity sums are 37 wherein at about 0.401nm wavelength place with in 0.334nm wavelength place impurity peaks intensity, second characteristic peak (0.449nm) intensity of smectite is the intensity of 53, two impurity peaks intensity sums less than second characteristic peak (0.449nm) of smectite.All other indexs are measured by existing smectite quality standard, and are all up to specification.Conclusion: judge by existing medicinal smectite quality standard, qualified.X ray diffracting spectrum judging standard by a kind of medicinal smectite of the present invention is judged, and is qualified.
Get commercially available dioctahedral smectite one bag, contain smectite 3g, add ethanol 60ml, stir, filter, 3 times repeatedly, remove auxiliary material, after the drying, be ground into fine powder, in the exsiccator of relative humidity 75%, placed about 12 hours when putting 20 ℃, measure the record collection of illustrative plates according to x-ray powder diffraction (Chinese Pharmacopoeia version appendix in 2005 IX F).X ray diffracting spectrum shows the characteristic spectral line of smectite at 1.492nm and 0.451nm wavelength place, locate to show the impurity peaks spectral line 0.408nm, 0.329nm equiwavelength in the collection of illustrative plates, impurity peaks intensity all is not higher than second characteristic peak (0.446nm wavelength place) of smectite, be respectively that 21,15 both intensity sums are 36 wherein at about 0.408nm wavelength place with in 0.329nm wavelength place impurity peaks intensity, second characteristic peak (0.451nm) intensity of smectite is the intensity of 49, two impurity peaks intensity sums less than second characteristic peak (0.448nm) of smectite.All other indexs are measured by existing smectite quality standard, and are all up to specification.Conclusion: judge by existing medicinal smectite quality standard, qualified.X ray diffracting spectrum judging standard by a kind of medicinal smectite of the present invention is judged, and is qualified.
Claims (6)
1, a kind of X ray diffracting spectrum judging standard of medicinal smectite, the characteristic spectral line that it is characterized in that smectite X-ray diffraction map is at about 1.5nm and about 0.45nm wavelength place, other impurity peaks intensity must not be higher than second characteristic peak (about 0.45nm wavelength place) of smectite in the collection of illustrative plates, and wherein two impurity peaks intensity sums at about 0.40nm wavelength place and about 0.33nm wavelength place must not be higher than second characteristic peak (about 0.45nm wavelength place) of smectite.
2, according to the X ray diffracting spectrum judging standard of a kind of medicinal smectite of claim 1, it is characterized in that the X ray diffracting spectrum assay method is: get smectite an amount of (about 3g), when putting 20 ℃ in the exsiccator of relative humidity 75%, placed about 12 hours, measure the record collection of illustrative plates according to x-ray powder diffraction (Chinese Pharmacopoeia version appendix in 2005 IX F).
3, according to the X ray diffracting spectrum judging standard of a kind of medicinal smectite of claim 1, it is characterized in that can be used for the X ray diffracting spectrum judging standard of smectite preparation, method is to get smectite preparation an amount of (containing smectite 3g approximately), solubilizer, stir, filter, remove auxiliary material, filter cake is after drying below 105 ℃, when putting 20 ℃ in the exsiccator of relative humidity 75%, placed about 12 hours, and measured, the record collection of illustrative plates according to x-ray powder diffraction (Chinese Pharmacopoeia version appendix in 2005 IXF).The characteristic spectral line of smectite X-ray diffraction map is at about 1.5nm and about 0.45nm wavelength place, other impurity peaks intensity must not be higher than second characteristic peak (about 0.45nm wavelength place) of smectite in the collection of illustrative plates, and wherein two impurity peaks intensity sums at about 0.40nm wavelength place and about 0.33nm wavelength place must not be higher than second characteristic peak (about 0.45nm wavelength place) of smectite.
4, according to the X ray diffracting spectrum judging standard of a kind of medicinal smectite of claim 1, the X ray diffracting spectrum judging standard that it is characterized in that the smectite preparation, can also get smectite preparation an amount of (containing smectite 3g approximately), be ground into fine powder, when putting 20 ℃ in the exsiccator of relative humidity 75%, placed about 12 hours, and measured, the record collection of illustrative plates according to x-ray powder diffraction (Chinese Pharmacopoeia version appendix in 2005 IX F).The characteristic spectral line of smectite X-ray diffraction map is at about 1.5nm and about 0.45nm wavelength place, in the collection of illustrative plates except that the auxiliary material peak, other impurity peaks intensity must not be higher than second characteristic peak (about 0.45nm wavelength place) of smectite, and wherein two impurity peaks intensity sums at about 0.40nm wavelength place and about 0.33nm wavelength place must not be higher than second characteristic peak (about 0.45nm wavelength place) of smectite.
5, according to the X ray diffracting spectrum judging standard of a kind of medicinal smectite of claim 3 or claim 4, it is characterized in that the smectite preparation comprises powder, tablet, capsule, granule, supensoid agent, gel, the clinical formulation commonly used of dispersing tablet.
6, according to the X ray diffracting spectrum judging standard of a kind of medicinal smectite of claim 3, it is characterized in that described solvent comprises the mixed liquor of methyl alcohol, Different concentrations of alcohol and the methyl alcohol of water, Different concentrations of alcohol, variable concentrations.
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| CN102607925A (en) * | 2012-03-06 | 2012-07-25 | 济南康众医药科技开发有限公司 | Method for detecting impurity content and category of medicinal montmorillonite by heavy-liquid separation method |
| CN102607985A (en) * | 2012-03-06 | 2012-07-25 | 济南康众医药科技开发有限公司 | Water separation method for detecting impurity content and impurity categories of medicinal montmorillonite |
| CN102607926A (en) * | 2012-03-06 | 2012-07-25 | 济南康众医药科技开发有限公司 | Method for detecting content and categories of montmorillonite impurities |
| CN102608197A (en) * | 2012-03-06 | 2012-07-25 | 济南康众医药科技开发有限公司 | Electrophoresis separation method for detecting impurity content and types of medical montmorillonite |
| CN104034743A (en) * | 2014-05-29 | 2014-09-10 | 南京中医药大学 | Method for establishing X-ray powder diffraction Fourier fingerprint spectrum of limonite, standard fingerprint spectrum and application of X-ray powder diffraction Fourier fingerprint spectrum |
| CN106872504A (en) * | 2017-04-28 | 2017-06-20 | 广西壮族自治区梧州食品药品检验所 | A kind of x-ray fluorescence analysis are discerned the false from the genuine the method for cinnabar |
| CN107179327A (en) * | 2017-07-12 | 2017-09-19 | 四川维奥制药有限公司 | A kind of quality determining method of montmorillonite |
| CN108490007A (en) * | 2018-06-04 | 2018-09-04 | 西南民族大学 | The method that subdigitate wormwood herb and subdigitate wormwood herb charcoal are distinguished using X-ray diffraction method |
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| CN102607925A (en) * | 2012-03-06 | 2012-07-25 | 济南康众医药科技开发有限公司 | Method for detecting impurity content and category of medicinal montmorillonite by heavy-liquid separation method |
| CN102607985A (en) * | 2012-03-06 | 2012-07-25 | 济南康众医药科技开发有限公司 | Water separation method for detecting impurity content and impurity categories of medicinal montmorillonite |
| CN102607926A (en) * | 2012-03-06 | 2012-07-25 | 济南康众医药科技开发有限公司 | Method for detecting content and categories of montmorillonite impurities |
| CN102608197A (en) * | 2012-03-06 | 2012-07-25 | 济南康众医药科技开发有限公司 | Electrophoresis separation method for detecting impurity content and types of medical montmorillonite |
| CN104034743A (en) * | 2014-05-29 | 2014-09-10 | 南京中医药大学 | Method for establishing X-ray powder diffraction Fourier fingerprint spectrum of limonite, standard fingerprint spectrum and application of X-ray powder diffraction Fourier fingerprint spectrum |
| CN106872504A (en) * | 2017-04-28 | 2017-06-20 | 广西壮族自治区梧州食品药品检验所 | A kind of x-ray fluorescence analysis are discerned the false from the genuine the method for cinnabar |
| CN107179327A (en) * | 2017-07-12 | 2017-09-19 | 四川维奥制药有限公司 | A kind of quality determining method of montmorillonite |
| CN109696377A (en) * | 2017-10-24 | 2019-04-30 | 中国石油化工股份有限公司 | The method of building sample cell gas atmosphere, sample analysis method and analysis instrument under gas atmosphere |
| CN108490007A (en) * | 2018-06-04 | 2018-09-04 | 西南民族大学 | The method that subdigitate wormwood herb and subdigitate wormwood herb charcoal are distinguished using X-ray diffraction method |
| CN108490007B (en) * | 2018-06-04 | 2021-02-26 | 西南民族大学 | Method for distinguishing artemisia rupestris L and artemisia rupestris L charcoal by adopting X-ray diffraction method |
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