CN107064190A - The improved method of asbestos component in a kind of identification medicine - Google Patents
The improved method of asbestos component in a kind of identification medicine Download PDFInfo
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- CN107064190A CN107064190A CN201610736669.6A CN201610736669A CN107064190A CN 107064190 A CN107064190 A CN 107064190A CN 201610736669 A CN201610736669 A CN 201610736669A CN 107064190 A CN107064190 A CN 107064190A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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Abstract
The invention belongs to trace mineral detection technique field, and in particular to the improved method of asbestos component in a kind of identification medicine.Its feature comprises the following steps：Sample is analyzed by X x ray diffractometer xs, reuses stereomicroscope and petrographic microscope is analyzed.The characteristic diffraction peak occurred according to different asbestos under the detection of X x ray diffractometer xs, and according to change of the different asbestos fibres using various optical phenomenas of the corresponding index-matching fluid under petrographic microscope, to judge the species of asbestos.Detect that the variety classes asbestos in medicine are more direct, accurate, quick with the method for the invention.
Description
Technical field
This method belongs to trace mineral detection field, is related to a kind of quick determination method of asbestos, more particularly in one kind
The improved method that asbestos are detected in state's pharmacopeia.
Background technology
Contain talcum powder in food ingredient in medicine Waterelon Frost Lozenges, contain west in such as certain Waterelon Frost Lozenges composition
Melon frost, borneol, peppermint oil dementholized, menthol；Auxiliary material is dextrin, sucrose, citric acid, magnesium stearate, talcum powder, food coloring, tangerine
Sub- essence, silica.
Due to talcum powder often with asbestos mineral symbiosis, the asbestos of trace may be carried in talcum powder used in throat lozenge
Fiber.
Asbestos (Asbestos) are a kind of mineral fibres, have serpentine asbestoid (chrysotile) and hornblend asbestoid (to have
Crocidolite, amosite, the tremolite, anthophyllite, actinolite).Because asbestos fibre is smaller, and it is readily suspended in air,
After being sucked by people, small asbestos fibre can enter the positions such as throat or alveolar, and canceration can be caused for a long time by sucking.If medicine
The talcum powder containing micro carcinogenic kind of asbestoid is used in production, long-term consumption can produce potentially hazardous to health.
The method of trace asbestos is based on Chinese Pharmacopoeia (version the 4th in 2015) in detection medicine at present.Chinese Pharmacopoeia
The scanning range of x-ray diffractometer is 10 ° -13 ° and 24 ° -26 ° in method, can meet the asbestos (chrysotile) of serpentine class
Characteristic peak is 12.05 ° ± 0.1 ° and 24.35 ° ± 0.1 ° of detection in 2 θ, but the asbestos of hornblend class, such as tremolite asbestos,
Its characteristic peak 2 θ be 10.55 ° ± 0.1 ° and 28.54 ° ± 0.1 °, its characteristic peak of amosite 2 θ be 10.62 ° ± 0.1 ° with
29.18 ° ± 0.1 ° etc., the scanning range in Chinese Pharmacopoeia method, can cause the missing inspection of asbestos fibre.
The angle of diffraction of X-ray diffractometer is usually 5 ° -70 ° in the detection method of asbestos, the meeting in this angular interval
There are many asbestos characteristic peaks.Some characteristic peaks are obvious, are difficult by the peak covering of host material.Therefore, patent applicant
When characteristic peak is referred to, all referring to obvious, and it is difficult by the peak of the peak influence of host material.
Figure 11 is the XRD diffraction patterns containing tremolite asbestos in talcum powder.Its characteristic peak is 10.55 ° and 28.54 °, still
It is difficult to be seen that there is obvious characteristic peak between 24 ° -26 ° of the angle of diffraction.
In the method detected now concerning asbestos, used instrument is powder x-ray diffraction (XRD) and polarized light microscopy
Mirror (PLM).And most of operations for only explaining XRD in method, and PLM parts explain very clear.Such as《Powder cosmetic and its
Asbestos assay method in raw material》(notice on providing asbestos assay method (tentative) in powder cosmetic and its raw material) (food
Medicine prison does Xu Han [2009] 136) (linkhttp://www.sda.gov.cn/WS01/CL0846/37316.html, link Date2016.07.05 also it is the immersion oil film-making using 1.550 in).When containing a variety of asbestos for a sample, it is impossible to full
Foot detection is required.
When being PLM, every kind of asbestos can all have different index-matching fluids, the corresponding index-matching fluid of such as chrysotile
For 1.550, the corresponding index-matching fluid of tremolite asbestos is 1.605, the corresponding index matching liquid level 1.700 of crocidolite
(refer to ISO22262-1：2012) etc..
Therefore, scanning range can not fully meet the detection of asbestos in medicine in Chinese Pharmacopoeia, and this method is penetrated using X-
The scanning range of line diffractometer is 5 ° -70 °, can fully meet the asbestos detection in medicine.
Asbestos fibre is judged by light microscope in another Chinese Pharmacopoeia, then is difficult to carry out area with other non-asbestos fibers
Go-on-go is surveyed；And then can accurately more identify asbestos fibre using stereomicroscope and petrographic microscope in the inventive method.
Asbestos have different optical properties, such as ductility, Extinction Characteristic, discrete dyeability under polarized light.Optics face
The discrete dyeability of the change of color, such as chrysotile is become carmetta horizontally by the blueness of vertical direction, and other non-
Asbestos fibre does not possess the optical property of the above.With《Chinese Pharmacopoeia》Asbestos compare cage in the detection medicine (such as throat lozenge) of method
System, directiveness are poor, are easily judged by accident in detection process, and detection cycle is longer, and it is quickly accurate often to meet client
True detection requirement.
The more preferable detection method about asbestos in medicine in pharmacopeia is not found in the literature at present.Therefore, set up a kind of
Quickly, accurately, conveniently and economic authentication method, be conducive to monitoring the presence of asbestos fibre in medicine, so as to ensure that medicine is pacified
Entirely.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of step simply, the method that a variety of asbestos can be detected simultaneously,
Pre-treatment is met simultaneously simple, quick, a variety of asbestos can be detected simultaneously.
To achieve the above object, the present invention takes following design：
Asbestos detection method comprises the following steps in the throat lozenge of the present invention：
Sample pre-treatments：
(1) by throat lozenge, calcination is ashed 1h in Muffle furnace, and the sample being ashed after cooling was ground into 200 mesh sieves
Son.
(2) the throat lozenge ash content after processing is prepared into upper x-ray diffractometer to be detected.The setting of x-ray diffractometer
Parameter：Tube voltage：40KV
Tube current：30mA
Sweep speed：1.2°/min
Scanning range：5°-70°
(3) sample is directly observed under stereomicroscope, finds asbestos fibre, fiber is picked out to be placed on tweezers contained
Have on the slide of index-matching fluid, covered, then carry out observation fibre optics property using petrographic microscope.
Figure of description
Fig. 1 is the X-ray diffraction standard drawing of chrysotile；
Fig. 2 is the X-ray diffraction standard drawing of amosite；
Fig. 3 is the X-ray diffraction standard drawing of blue or green (indigo plant) asbestos；
Fig. 4 is the X-ray diffraction standard drawing of the tremolite or actinolite；
Fig. 5 is the X-ray diffraction standard drawing of anthophyllite；
Fig. 6 is talcum powder X-ray diffractogram in embodiment；
Fig. 7 is the sample X-ray diffractogram in embodiment 1；
Fig. 8 is the sample X-ray diffractogram in embodiment 2；
Fig. 9 a are the petrographic microscope figures of asbestos ductility in embodiment 1；
Fig. 9 b are the petrographic microscope figures of asbestos Extinction Characteristic in embodiment 1；
Fig. 9 c are the discrete chromatic petrographic microscope figures of asbestos in embodiment 1；
Figure 10 a are the petrographic microscope figures of asbestos ductility in embodiment 2；
Figure 10 b are the petrographic microscope figures of asbestos Extinction Characteristic in embodiment 2；
Figure 10 c are the discrete chromatic petrographic microscope figures of asbestos in embodiment 2；
Figure 11 is the X-ray diffractogram containing tremolite sample.
Embodiment
Below in conjunction with specific embodiment, the present invention is expanded on further.These embodiments be merely to illustrate the present invention and without
In limitation the scope of the present invention.The experimental method of unreceipted actual conditions in the following example, generally according to normal condition or is pressed
According to the condition proposed by manufacturer.Unless otherwise defined, all specialties used in text are ripe with this area with scientific words
Practice meaning known to personnel identical.In addition, any method similar or impartial to described content and material all can be applied to
In the inventive method.Preferable implementation described in text only presents a demonstration with material to be used.
Embodiment 1
Sample source：Commercially available Waterelon Frost Lozenges
1.1 instruments and reagent
X-ray diffractometer：TD Technologies Co., Ltd. TD-3500
Stereomicroscope：Olympus SZ61
Petrographic microscope：Come card DM2700P
Asbestos standard items：Chrysotile, amosite, crocidolite, anthophyllite, the tremolite, actinolite
Index-matching fluid：1.550±0.005、1.605±0.005、1.630±0.005、1.670±0.005、
1.700±0.005。
1.2 sample pretreatment
By throat lozenge, 450 DEG C of ashing one more than hour, the sample being ashed after cooling were ground in Muffle furnace
200 mesh sieve.
1.3 instrumental conditions
X-ray diffractometer：
Tube voltage：40KV,
Tube current：30mA
Sweep speed：1.2°/min
Scanning range：5°-70°
Petrographic microscope：
100-400 times of multiplication factor
Polarised light
2 sample detection steps
The detection of 2.1X- x ray diffractometer xs：Throat lozenge powder after pre-treatment is put into sample cell and flattened, Ran Hou
The sample stage that sample cell equipped with throat lozenge powder is put into instrument is detected.
2.2 the detection of petrographic microscope：
2.2.1 sample is observed under stereomicroscope, finds asbestos fibre, and taken out and be put into containing refractive index with tweezers
On the slide of matching fluid, then covered.
2.2.2 the print in 2.2.1 steps is placed on progress observation checking on the sample stage of petrographic microscope, if can see
Observe the optical properties such as ductility, Extinction Characteristic, birefringence, pleochroism, the discrete dyeability of asbestos fibre.
3 data results are analyzed
3.1 Samples EXAMPLEs 1 (Fig. 7 is shown in x-ray diffractometer analysis).In Fig. 7 XRD diffraction pattern, patent applicant can
To analyze in addition to the characteristic peak of talcum powder (Fig. 6) in throat lozenge, also other obvious peaks, wherein 2 θ angles at 12.05 ° and
24.35 ° nearby there is obvious characteristic peak, go control by the X-ray diffractogram (Fig. 1) with asbestos, finding can in the throat lozenge
Chrysotile can be contained.Then detected using petrographic microscope, look for chrysotile asbestos fibre.Due to the refraction of chrysotile asbestos fibre
Rate is 1.550 at 20 DEG C, so to use the index-matching fluid that refractive index is 1.550 ± 0.005 to carry out film-making, Ran Hou
Observed under petrographic microscope.It is observed that the optics such as the form of its chrysotile, ductility, Extinction Characteristic, discrete dyeability
Property.See Fig. 9.
Comprehensive profile information patent applicant is found that the characteristic peak of chrysotile in XRD diffraction pattern, and aobvious in polarisation
The various optical property color changes of asbestos fibre and chrysotile are found that under micro mirror in refractive index is 1.550 matching fluid,
As fiber becomes au bleu by red under the conditions of ductility；Fiber is in 90 ° of delustrings under extinction conditions；The fiber under discrete dyeing condition
In vertical direction in blueness, in the horizontal direction in carmetta.Comprehensive XRD diffraction pattern and petrographic microscope atlas analysis, the west
Contain chrysotile in melon frost throat lozenge.
Embodiment 2
Sample source：Commercially available Waterelon Frost Lozenges sample 2
Instrument and reagent, sample pretreatment, instrumental conditions and sample detection step be the same as Example 1.
Data result is analyzed
Fig. 8 is shown in x-ray diffractometer analysis.In Fig. 8 XRD diffraction pattern, patent applicant can be analyzed except throat lozenge
Outside the characteristic peak of middle talcum powder (Fig. 6), also other obvious peaks, wherein 2 θ angles occur substantially near 10.54 ° and 28.54 °
Characteristic peak, goes control by the X-ray diffractogram (Fig. 4) with asbestos, finds that tremolite asbestos may be contained in the throat lozenge.So
Tested and analyzed afterwards using petrographic microscope, look for tremolite fiber.Because the refractive index of tremolite fiber is at 20 DEG C
For 1.605, so patent applicant will use the index-matching fluid that refractive index is 1.605 ± 0.005 to carry out film-making, Ran Hou
Observed under petrographic microscope.It is observed that the optics such as the form of its chrysotile, ductility, Extinction Characteristic, discrete dyeability
Property.Below figure 10.
Comprehensive profile information patent applicant is found that the characteristic peak of tremolite asbestos in XRD diffraction pattern, and inclined
The various optical property face of asbestos fibre and tremolite asbestos are found that under light microscope in refractive index is 1.605 matching fluid
Fiber becomes au bleu by red under the conditions of color change, such as ductility；Fiber has individual low-angle delustring under extinction conditions；In discrete dye
Fiber is in blueness in vertical direction under the conditions of color, in the horizontal direction in rufous.Comprehensive XRD diffraction pattern and petrographic microscope figure
Contain tremolite asbestos in analysis of spectrum, the throat lozenge.
Similarly, patent applicant can also analyze antophyllite, actinolite asbestos, amosite, the crocidolite in sample
Deng.
Above-described embodiment is used for illustrative purposes only, and is not limitation of the present invention, and this patent can not only be fitted
For Waterelon Frost Lozenges, other medicines that raw material or additive are done with talcum powder are also applied for, about the general of technical field
Logical technical staff, without departing from the present invention, can be therefore all equivalent so that various changes can be made and modification
Technical scheme should also belong to scope of the invention, and scope of patent protection of the invention is limited by each claim.
Claims (3)
1. a kind of improved method for identifying asbestos component in medicine, comprises the following steps：
A) sample pre-treatments：Sample is ashed to a hour in Muffle furnace, the sample being ashed after cooling was ground 200
Mesh sieve；
B) X-ray diffractometer detection is carried out；Treated ash content powder is subjected to compressing tablet process, then upper X-ray diffractometer, X
X ray diffractometer x condition：Tube voltage：40KV, tube current：30mA, sweep speed：1.2 °/min, scanning range：5°-70°.
C) treated ash content powder is subjected to stereomicroscope and petrographic microscope is tested and analyzed：Sample is directly stereoscopic micro-
Microscopic observation, finds asbestos fibre, fiber is picked out with tweezers and is placed on the slide containing index-matching fluid, is closed the lid
Slide, then carries out observation fibre optics property using petrographic microscope.
2. a kind of improved method for identifying asbestos component in medicine according to claim 1, it is characterised in that use refraction
Rate matching fluid.
3. a kind of improved method for identifying asbestos component in medicine according to claim 1, it is characterised in that with reference to X-ray
Diffractometer, stereomicroscope and petrographic microscope identify the species of asbestos fibre.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610736669.6A CN107064190A (en) | 2016-08-26 | 2016-08-26 | The improved method of asbestos component in a kind of identification medicine |
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| CN201610736669.6A CN107064190A (en) | 2016-08-26 | 2016-08-26 | The improved method of asbestos component in a kind of identification medicine |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108445028A (en) * | 2018-03-16 | 2018-08-24 | 中国检验检疫科学研究院 | Polarized light microscopy-X-ray diffraction method of asbestos in a kind of qualitative detection electronic product |
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| CN102778467A (en) * | 2012-07-30 | 2012-11-14 | 中国检验检疫科学研究院 | Method for detecting harmful substances of asbestos |
| CN103076348A (en) * | 2012-12-29 | 2013-05-01 | 上海华碧检测技术有限公司 | Method for detecting content of asbestos in sample |
| CN103323470A (en) * | 2013-01-13 | 2013-09-25 | 赵景红 | Toilet powder and detection method of asbestos in talcum powder |
| CN103733048A (en) * | 2011-08-12 | 2014-04-16 | 国立大学法人广岛大学 | Method for detecting asbestos |
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2016
- 2016-08-26 CN CN201610736669.6A patent/CN107064190A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103733048A (en) * | 2011-08-12 | 2014-04-16 | 国立大学法人广岛大学 | Method for detecting asbestos |
| CN102589962A (en) * | 2012-01-18 | 2012-07-18 | 济南康众医药科技开发有限公司 | Method for detecting mineral fiber of montmorillonite by water enrichment method |
| CN102778467A (en) * | 2012-07-30 | 2012-11-14 | 中国检验检疫科学研究院 | Method for detecting harmful substances of asbestos |
| CN103076348A (en) * | 2012-12-29 | 2013-05-01 | 上海华碧检测技术有限公司 | Method for detecting content of asbestos in sample |
| CN103323470A (en) * | 2013-01-13 | 2013-09-25 | 赵景红 | Toilet powder and detection method of asbestos in talcum powder |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108445028A (en) * | 2018-03-16 | 2018-08-24 | 中国检验检疫科学研究院 | Polarized light microscopy-X-ray diffraction method of asbestos in a kind of qualitative detection electronic product |
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Application publication date: 20170818 |