CN112129798A - Method for measuring content of native copper in Chinese patent medicine - Google Patents
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 33
- 239000010949 copper Substances 0.000 title claims abstract description 33
- 239000003814 drug Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000006185 dispersion Substances 0.000 claims abstract description 12
- 238000002795 fluorescence method Methods 0.000 claims abstract 3
- 239000003826 tablet Substances 0.000 claims description 12
- 230000003287 optical effect Effects 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 239000002775 capsule Substances 0.000 claims description 7
- 239000011248 coating agent Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
- 229910052683 pyrite Inorganic materials 0.000 claims description 5
- 239000006187 pill Substances 0.000 claims description 4
- 230000003595 spectral effect Effects 0.000 claims description 4
- 229910052960 marcasite Inorganic materials 0.000 claims description 3
- 229910019589 Cr—Fe Inorganic materials 0.000 claims description 2
- 229910052745 lead Inorganic materials 0.000 claims description 2
- 238000004458 analytical method Methods 0.000 abstract description 10
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 abstract description 9
- 238000004846 x-ray emission Methods 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 14
- 238000005259 measurement Methods 0.000 description 12
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 11
- 210000003205 muscle Anatomy 0.000 description 5
- 239000008280 blood Substances 0.000 description 4
- 210000004369 blood Anatomy 0.000 description 4
- 230000017531 blood circulation Effects 0.000 description 4
- 229940079593 drug Drugs 0.000 description 4
- 230000001737 promoting effect Effects 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 244000061520 Angelica archangelica Species 0.000 description 2
- 235000003717 Boswellia sacra Nutrition 0.000 description 2
- 240000007551 Boswellia serrata Species 0.000 description 2
- 235000012035 Boswellia serrata Nutrition 0.000 description 2
- 239000004863 Frankincense Substances 0.000 description 2
- 235000001287 Guettarda speciosa Nutrition 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000004737 colorimetric analysis Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000029087 digestion Effects 0.000 description 2
- 238000004993 emission spectroscopy Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 235000008216 herbs Nutrition 0.000 description 2
- 238000009616 inductively coupled plasma Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000691 measurement method Methods 0.000 description 2
- 238000000120 microwave digestion Methods 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical group [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 2
- 239000011028 pyrite Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000002040 relaxant effect Effects 0.000 description 2
- 230000008961 swelling Effects 0.000 description 2
- 210000002435 tendon Anatomy 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- DTGKSKDOIYIVQL-WEDXCCLWSA-N (+)-borneol Chemical compound C1C[C@@]2(C)[C@@H](O)C[C@@H]1C2(C)C DTGKSKDOIYIVQL-WEDXCCLWSA-N 0.000 description 1
- REPVLJRCJUVQFA-UHFFFAOYSA-N (-)-isopinocampheol Natural products C1C(O)C(C)C2C(C)(C)C1C2 REPVLJRCJUVQFA-UHFFFAOYSA-N 0.000 description 1
- 208000010392 Bone Fractures Diseases 0.000 description 1
- 241000131329 Carabidae Species 0.000 description 1
- 244000020518 Carthamus tinctorius Species 0.000 description 1
- 235000003255 Carthamus tinctorius Nutrition 0.000 description 1
- 240000007311 Commiphora myrrha Species 0.000 description 1
- 235000006965 Commiphora myrrha Nutrition 0.000 description 1
- 235000007265 Myrrhis odorata Nutrition 0.000 description 1
- 244000131316 Panax pseudoginseng Species 0.000 description 1
- 235000003181 Panax pseudoginseng Nutrition 0.000 description 1
- 244000299790 Rheum rhabarbarum Species 0.000 description 1
- 235000009411 Rheum rhabarbarum Nutrition 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- NFMAZVUSKIJEIH-UHFFFAOYSA-N bis(sulfanylidene)iron Chemical compound S=[Fe]=S NFMAZVUSKIJEIH-UHFFFAOYSA-N 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- 229940116229 borneol Drugs 0.000 description 1
- CKDOCTFBFTVPSN-UHFFFAOYSA-N borneol Natural products C1CC2(C)C(C)CC1C2(C)C CKDOCTFBFTVPSN-UHFFFAOYSA-N 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- DTGKSKDOIYIVQL-UHFFFAOYSA-N dl-isoborneol Natural products C1CC2(C)C(O)CC1C2(C)C DTGKSKDOIYIVQL-UHFFFAOYSA-N 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910000339 iron disulfide Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 239000004328 sodium tetraborate Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910052569 sulfide mineral Inorganic materials 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 229940126680 traditional chinese medicines Drugs 0.000 description 1
- 230000000472 traumatic effect Effects 0.000 description 1
- 230000008736 traumatic injury Effects 0.000 description 1
- 238000004876 x-ray fluorescence Methods 0.000 description 1
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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
- G01N23/22—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 measuring secondary emission from the material
- G01N23/223—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 measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
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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
- G01N23/22—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 measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
- G01N2223/076—X-ray fluorescence
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/10—Different kinds of radiation or particles
- G01N2223/101—Different kinds of radiation or particles electromagnetic radiation
- G01N2223/1016—X-ray
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention belongs to the technical field of Chinese patent medicine content determination, and particularly relates to a content determination method of native copper in Chinese patent medicine, which comprises the following steps: taking the Chinese patent medicine, and carrying out quantitative determination on all elements by adopting an energy dispersion type X fluorescence method. The method for measuring the native copper in the Chinese patent medicine by the energy dispersion X-ray fluorescence spectrometry has the advantages of high precision and good repeatability, and the measured value is close to the reference value measured by the ICP-OES method. Has the advantages of simple operation, high analysis speed (6.6 min for 1 sample), no need of pretreatment, realization of nondestructive analysis, and the like.
Description
Technical Field
The invention belongs to the technical field of Chinese patent medicine content determination, and particularly relates to a method for determining the content of native copper in Chinese patent medicines.
Background
Pyritum is pyrite of pyrite family, which is sulfide mineral and mainly contains iron disulfide (FeS)2) The traditional Chinese medicine is a common mineral traditional Chinese medicine, has the functions of removing blood stasis and relieving pain and reuniting bones, is used for treating traumatic injury, fracture of bones and muscles and pain due to blood stasis and swelling, is often combined with other traditional Chinese medicines to prepare a Chinese patent medicine, and is clinically used for diseases such as traumatic swelling and pain. FeS2Is combined by covalent bond and is difficult to dissolve in dilute acid, and the content determination of the native copper in the Chinese patent medicine is only reported. A paper published by the Hujun et al, namely a research on measuring the content of total iron in native copper in a blood circulation-promoting and pain-relieving capsule (the Proc of Jiangxi college of traditional Chinese medicine, 2003), adopts a colorimetric method to measure the content of native copper in a Chinese patent medicine after the high-temperature digestion under severe conditions. The method has the advantages of low sensitivity, large sampling quantity, fussy operation and larger error. On the other hand, the Chinese patent medicine has complex matrix and needs to be cleared up, so that the pretreatment is complex, the time consumption is long, and the environment is polluted. The energy dispersive X-ray fluorescence spectroscopy (EDX) has the advantages of simple operation, high analysis speed, simultaneous detection of multiple elements, realization of nondestructive analysis and the like. At present, the analysis of EDX for Chinese patent medicines is not reported.
Disclosure of Invention
The invention aims to provide a method for measuring the content of native copper in Chinese patent medicine, and the invention adopts an energy dispersion X-ray fluorescence method to establish a rapid nondestructive analysis method for native copper in Chinese patent medicine, thereby providing an accurate and feasible detection means for quality control of the Chinese medicine containing native copper.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for measuring the content of native copper in Chinese patent medicine comprises the following steps:
removing the coating/capsule shell of the sample, placing the sample in an automatic sample injector of an energy dispersion type X fluorescence spectrometer, or directly placing the sample in the automatic sample injector of the energy dispersion type X fluorescence spectrometer, and measuring the spectral line intensity of each element;
Ti-U element: a collimator: 10mm, atmosphere: vacuum, voltage 50kV, current 18 uA-Auto, scanning range 4.00-35.00, scanning time 60s, and dead time ratio 30%;
Al-Sc elements: a collimator: 10mm, atmosphere: vacuum, voltage 15kV, current 137 uA-Auto, scanning range 0.00-4.40, scanning time 60s, and dead time proportion 29%;
S-Ca element: a collimator: 10mm, atmosphere: vacuum, voltage 15kV, current 222 uA-Auto, optical filter # 2, scanning range 2.10-4.10, scanning time 60s and dead time proportion 30%;
Cr-Fe element: a collimator: 10mm, atmosphere: vacuum, voltage 50kV, current 34 uA-Auto, optical filter #3, scanning range of 5.00-7.00, scanning time 57s and dead time proportion of 30 percent;
Zn-As, Pb element: a collimator: 10mm, atmosphere: vacuum, voltage 50kV, current 352 uA-Auto, optical filter #4, scanning range 8.50-14.50, scanning time 54s and dead time proportion 30 percent;
Ru-Sb element: a collimator: 10mm, atmosphere: vacuum, voltage 50kV, current 1000 uA-Auto, optical filter #1, scanning range 18.50-28.00, scanning time 60s and dead time proportion 9%;
according to the line intensity of each element, combining CHO equilibrium and FeS2And (5) calculating to obtain the content of the native copper in the sample. Preferably, the Chinese patent medicine is powder, pills, tablets or capsules. The powder and pill can be directly measured, the tablet can be measured without removing or removing coating, and the capsule can be measured by taking the content.
Compared with the prior art, the invention has the technical advantages that:
the method for measuring the native copper in the Chinese patent medicine by the energy dispersion X-ray fluorescence spectrometry has the advantages of high precision and good repeatability, and the measured value is close to the reference value measured by the ICP-OES method.
The invention has the advantages of simple operation, high analysis speed (6.6 min for 1 sample), no need of pretreatment, realization of nondestructive analysis and the like.
The invention does not need to adopt solvent for digestion, does not pollute the environment and is beneficial to environmental protection; the test sample does not need to be crushed, the content can be directly measured, the test preparation time is saved, and the measurement result is accurate.
Drawings
FIG. 1EDX method for determining Pyritum content in tablet for relieving rigidity of muscles and relieving pain;
FIG. 2 shows a regression model of correlation between EDX measurement of Pyritum and ICP-OES measurement in SHUJINDINGTONG tablet;
FIG. 3 is a regression model of correlation between EDX measurement of Pyritum and ICP-OES measurement in the blood circulation promoting and pain relieving tablet.
Detailed Description
The invention is described in further detail below with reference to the figures and the detailed description.
Example a content determination of Pyritum in tablet for relaxing muscles and tendons and relieving pain
1. Measurement method
Taking the tablet for relieving rigidity of muscles and relieving pain, removing or not removing coating, placing in an automatic sample injector as shown in figure 1, quantitatively determining the intensity of each element by using Shimadzu EDX-7000 energy dispersion type X fluorescence spectrometer, and combining CHO balance and FeS according to the intensity of each element spectral line2And (5) calculating to obtain the content of the native copper in the sample. Analysis time 6.6min, instrument parameters set as table 1 below:
TABLE 1 energy dispersive X-ray fluorescence test conditions
2. Specificity test
Taking ground beetle, safflower, rhizoma drynariae, angelica, frankincense, myrrh, rhubarb and borax, preparing a negative sample lacking the native copper according to the proportion of the prescription of the muscle-relaxing pain-relieving tablet, and determining according to the method, wherein FeS is not detected2The other herbs have no interference to the determination of native copper in the product.
3. Precision test
Continuously measuring a part of the sample for 6 times to obtain Pyritum (in FeS form)2Calculated) average content of 25.03 percent and RSD of 1.14％。
4. Repeatability test
Taking the same batch of samples, preparing 6 test samples in parallel, and measuring the native copper (FeS)2Calculated) the average content was 24.95% and the RSD was 2.27%.
5. Accuracy test
Taking the tablet for relaxing muscles and tendons and relieving pain, removing the coating, grinding, precisely weighing 0.5g, adding 5.0mL of nitric acid, performing microwave digestion, removing acid, cooling, adding water to constant volume to 20.0mL, and determining the reference value by inductively coupled plasma emission spectrometry (ICP-OES). The instrument parameters are as follows: plasma radio frequency power 1300W, sampling depth 15.0mm, plasma gas flow 15.0 L.min-1Auxiliary air flow of 0.2 L.min-1The flow rate of the atomizing gas is 0.8 L.min-1And, measuring wavelength: fe 239.5 nm. Reference value between EDX measured value and ICP-OES measured value (the content of native copper is FeS)2Meter) is shown in fig. 2 (where the sample test data points coincide). As can be seen from fig. 2, the EDX measurements for the 13 samples were close to the reference value with an average relative deviation of 5.83%.
6. Measurement results
Taking 13 batches of 5 manufacturers, determining the native copper (by FeS)2Calculated) are shown in table 2 below:
TABLE 2 measurement results of samples from different manufacturers and different batches
| Serial number | Manufacturer of the product | Batch number | Measured value% |
| 1 | A | 190703 | 1.13 |
| 2 | A | 191002 | 1.20 |
| 3 | A | 191101 | 1.33 |
| 4 | B | 191201 | 25.35 |
| 5 | B | 191103 | 49.04 |
| 6 | B | 191204 | 38.78 |
| 7 | C | 990160 | 24.95 |
| 8 | C | 990161 | 25.18 |
| 9 | C | 990162 | 22.76 |
| 10 | D | 20190310 | 11.97 |
| 11 | D | 20191108 | 18.37 |
| 12 | D | 20190802 | 11.80 |
| 13 | E | 191104 | 73.77 |
The results show that the content of samples from different manufacturers has obvious difference. The conventional methods such as colorimetry, titration, ICP-OES and the like are used for measuring the content of the native copper in the Chinese patent medicine, so that the defects of complex operation, long consumed time and the like exist, and the content measurement item of the native copper with the medicinal taste of the prescription is not specified in the standard of the muscle-relaxing pain-relieving tablet, so that the feeding control of the supposition enterprise on the native copper is not standard. The content of the samples of the batch 3 of the A manufacturer is far lower than that of other samples, and the feeding amount is presumed to be obviously insufficient. B. In the D enterprise, the content of different batches of samples of the same manufacturer is different, which indicates that the quality of raw materials or the feeding condition of the samples is different greatly. The content of the samples of the enterprise E is far higher than that of other samples, and the feeding is presumed to be obviously higher or the feeding of other medicines except for the native copper is lower. And D, the content of the 3 batches of samples of the enterprise is close, which shows that the raw material quality is stable and the production management is standard. Therefore, the rapid, simple, convenient and accurate technical advantages of the invention are beneficial to the standard feeding of pharmaceutical manufacturing enterprises, and can provide powerful technical support for quality supervision of native copper-containing Chinese patent medicines.
EXAMPLE two determination of Pyritum content in blood circulation promoting and pain relieving powder
1. Measurement method
Taking the powder for promoting blood circulation and relieving pain, placing in an automatic sample injector, quantitatively determining the intensity of each element by adopting Shimadzu EDX-7000 energy dispersion type X fluorescence spectrometer, and combining CHO balance and FeS according to the spectral line intensity of each element2And (5) calculating to obtain the content of the native copper in the sample. Analysis time 6.6min, instrument parameters set as table 3 below:
TABLE 3 energy dispersive X-ray fluorescence test conditions
2. Specificity test
Preparing a negative sample lacking the native copper from the angelica, the pseudo-ginseng, the frankincense, the borneol and the ground beeltle according to the proportion of the prescription of the powder for activating blood and relieving pain, and determining according to a method, wherein FeS is not detected2The other herbs have no interference to the determination of native copper in the product.
3. Precision test
Continuously measuring a part of the sample for 6 times to obtain Pyritum (in FeS form)2Calculated) the average content was 7.67%, and the RSD was 1.55%.
4. Repeatability test
Taking the same batch of samples, preparing 6 test samples in parallel, and measuring the native copper (FeS)2Calculated) the average content was 7.73% and the RSD was 2.64%.
5. Accuracy of
Taking powder for promoting blood circulation and relieving pain, grinding, precisely weighing 0.5g, adding 5.0mL of nitric acid, performing microwave digestion, removing acid, cooling, adding water to constant volume to 20.0mL, and determining reference value by inductively coupled plasma emission spectrometry (ICP-OES). The instrument parameters are as follows: plasma RF power 1300W, sampling depth of 15.0mm, and plasma gas flow of 15.0L min-1Auxiliary air flow of 0.2 L.min-1The flow rate of the atomizing gas is 0.8 L.min-1And, measuring wavelength: fe 239.5 nm. Reference value between EDX measured value and ICP-OES measured value (the content of native copper is FeS)2Meter) is shown in fig. 3. As can be seen from fig. 3, the EDX measurements for the samples were close to the reference values with an average relative deviation of 4.56%.
6. Measurement results
Taking 9 batches of samples from 3 manufacturers, determining the samples according to the law, and obtaining the native copper (by FeS)2Calculated) are shown in table 4 below:
TABLE 4 measurement results of samples from different manufacturers
| Serial number | Manufacturer of the product | Batch number | Measured value% |
| 1 | A | 180301 | 7.73 |
| 2 | A | 180303 | 7.26 |
| 3 | A | 180305 | 7.51 |
| 4 | B | 170809 | 6.45 |
| 5 | B | 171014 | 6.03 |
| 6 | B | 171207 | 6.87 |
| 7 | C | 17040112 | 8.21 |
| 8 | C | 17100112 | 8.04 |
| 9 | C | 17110134 | 8.33 |
The method can be realized by upper and lower limit values and interval values of intervals of process parameters (such as temperature, time and the like), and embodiments are not listed.
Conventional technical knowledge in the art can be used for the details which are not described in the present invention.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and are not limited. Although the present invention has been described in detail with reference to the embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (2)
1. A method for measuring the content of native copper in Chinese patent medicine comprises the following steps:
taking the Chinese patent medicine, and carrying out quantitative determination on the full-element spectral line intensity by adopting an energy dispersion type X fluorescence method;
the energy dispersion type X fluorescence method specifically comprises the following steps:
Ti-U element: a collimator: 10mm, atmosphere: vacuum, voltage 50kV, current 18 uA-Auto, scanning range 4.00-35.00, scanning time 60s, and dead time ratio 30%;
Al-Sc elements: a collimator: 10mm, atmosphere: vacuum, voltage 15kV, current 137 uA-Auto, scanning range 0.00-4.40, scanning time 60s, and dead time proportion 29%;
S-Ca element: a collimator: 10mm, atmosphere: vacuum, voltage 15kV, current 222 uA-Auto, optical filter #2, scanning range 2.10-4.10, scanning time 60s and dead time proportion 30%;
Cr-Fe element: a collimator: 10mm, atmosphere: vacuum, voltage 50kV, current 34 uA-Auto, optical filter #3, scanning range of 5.00-7.00, scanning time 57s and dead time proportion of 30 percent;
Zn-As, Pb element: a collimator: 10mm, atmosphere: vacuum, voltage 50kV, current 352 uA-Auto, optical filter #4, scanning range 8.50-14.50, scanning time 54s and dead time proportion 30 percent;
Ru-Sb element: a collimator: 10mm, atmosphere: vacuum, voltage 50kV, current 1000 uA-Auto, optical filter #1, scanning range 18.50-28.00, scanning time 60s and dead time proportion 9%;
according to the line intensity of each element, combining CHO equilibrium and FeS2Molecular formula, calculated to obtain the molecular formula ofNatural copper content.
2. The method for measuring the content of claim 1, wherein the Chinese patent medicine is powder, pill, tablet or capsule;
when the Chinese patent medicine is a tablet or a capsule, removing the coating or the capsule shell of the sample, and placing the sample in an automatic sample injector of an energy dispersion type X fluorescence spectrometer;
when the Chinese patent medicine is powder or pill, the Chinese patent medicine is directly placed in an automatic sample injector of an energy dispersion type X fluorescence spectrometer.
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