CN107976481A - The detection method of scandium content in a kind of Chinese medicine - Google Patents
The detection method of scandium content in a kind of Chinese medicine Download PDFInfo
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Abstract
The invention discloses a kind of detection method of scandium content in Chinese medicine, analyzed using inductively coupled plasma mass spectrometry, its detecting step includes：（1）The preparation of series standard solution；（2）The preparation of inner mark solution；（3）The preparation of sample solution；（4）Carry out inductivity coupled plasma mass spectrometry（ICP‑MS）Analysis；（5）Result is calculated.The method of the invention is easy to operate, fast and easy, and detection efficiency is high, and accuracy is high, and precision is high, and with good stability and reappearance.The scope of application of Chinese medicine heavy metal analysis platform is expanded, can better ensure that the quality safety of Chinese medicine, technological reserve is provided for scandium assay in Chinese medicine.
Description
Technical field
The present invention relates to medicine detection field, the detection method of scandium content specifically in a kind of Chinese medicine.
Background technology
Residue of heavy metals and harmful elements as one of Chinese medicine exogenous pollution thing, always affect the quality of Chinese medicine with
And both at home and abroad to the impression of traditional Chinese medicine.For this reason, China formulates《Medicinal plant and preparation green professional standard》、《Chinese Pharmacopoeia》
Etc. standard, the heavy-metal residual of medicinal plant and medicinal material is controlled so as to ensure quality of medicinal material.From existing document report
And from the point of view of national standard, majority research concentrates on five lead, arsenic, mercury, cadmium, copper elements, and phase is studied in the detection of other elements
To less, while also lack corresponding data accumulation.
Scandium（Sc）It is a kind of rare earth element, the content in the earth's crust is few, and only 0.0005%.Since its content is extremely low,
Internal standard element is typically used as when measuring Residue of heavy metals and harmful elements using ICP-MS methods, is rarely had in existing document in detection
The report of scandium Sc contents in medicinal material.
The correlation technique of scandium content detection is also related in open source literature at present, here is to retrieve relevant patent text
Offer：
1st, Chinese patent：The assay method of scandium content in steel；Application number：01610731169.3；The applying date：2016-08-26；
Applicant：NeiMenggu BaoGang GangLian Co., Ltd；Summary：The invention discloses a kind of measure side of scandium content in steel
Method, including：Weigh steel sample and dissolved with nitration mixture and sample test solution is made, blank test is done in companion；In selected running parameter
Under, measure scandium working curve standard solution and sample test solution at the same time using icp ms；In measure scandium work
When composition line standard solution and sample test solution, it is measured by internal standard element of rhodium, the measured value of sample test solution subtracts blank value
To be tested the actual value of steel sample.The present invention have the advantages that it is easy to operate quickly, high sensitivity, accuracy it is high, meet
The demand of research and production.
2nd, Chinese patent：Gallium and the assay method of scandium content in blast furnace dust；Application number：201310225789.6；Application
Day： 2013-06-07；Applicant：Wuhan Iron And Steel Group Kunming Iron ＆ Steel Co., Ltd；Summary：The present invention provides a kind of blast furnace cigarette
Gallium and the assay method of scandium content in dirt, including measure test liquid with conventional inductively coupled plasma atomic emission spectrometry
The intensity of spectral line, corresponding gallium and scandium content value, its feature are obtained in the standard working curve of gallium and scandium according to the intensity of spectral line
It is that test liquid is made by the following steps：Sodium hydroxide high-temperature fusion sample, the sample hot water of melting are added in the sample
Lysate is leached to obtain, test solution is acidified with the sodium hydroxide pellets thing in dissolving with hydrochloric acid lysate, then with hydrochloric acid, obtains sample to be tested
Liquid.After the method for the present invention sample dissolution, you can gallium and scandium content in blast furnace dust are directly measured, it is not only easy to operate, but also survey
Fixed gallium and scandium content accuracy rate are high, its measurement result has good stability, reappearance and accuracy, is entirely capable of meeting daily
Measure gallium and the needs of scandium content in blast furnace dust.
The content of the invention
The purpose of the present invention is to expand the scope of application of Chinese medicine heavy metal and harmful element detection platform, ensure Chinese medicine
A kind of quality safety of material, there is provided the detection method of scandium content in Chinese medicine.
The present invention is achieved through the following technical solutions：
The detection method of scandium content, comprises the following steps in a kind of Chinese medicine：
（1）The preparation of series standard solution：Precision draws scandium single element titer（1000 mg·L-1）Add 2% salpeter solution dilute
Release, it is respectively 0.1 μ gL that scandium concentration, which is made,-1、0.5μg·L-1、1μg·L-1、5μg·L-1、10μg·L-1Series standard it is molten
Liquid.
（2）The preparation of inner mark solution：Precision is drawn germanium standard solution and is put in right amount in measuring bottle, adds 5% salpeter solution to be configured to dense
Spend for 500 μ gL-1Inner mark solution.
（3）The preparation of sample solution：Sample 0.4~the 0.8g for being ground into coarse powder is taken, it is accurately weighed, put in counteracting tank,
It is 7~8 to add volume ratio：0.5~1 nitrate acid and hydrofluoric acid mixed acid, mixes in postposition microwave dissolver and is carried out by certain procedures
Resolution；Let cool after resolution, put and catch up with sour frame 125~135 DEG C when catching up with acid 2~3 small, let cool to room temperature, be transferred to 25ml capacity
In bottle, wash counteracting tank 3~5 times with 2% salpeter solution of volumetric concentration, be diluted to scale, you can obtain sample solution.
（4）Carry out inductivity coupled plasma mass spectrometry（ICP-MS）Analysis：It is accurate respectively to draw series standard solution and sample
Product solution, injects icp ms, analysis measure is carried out according to certain condition.
（5）Result is calculated：Scandium content is obtained by standard curve.
The micro-wave digestion program is：Using temperature programming, 1030~1800W of power, 20~25min of time-to-climb,
190 DEG C of 20~25min of holding.
The inductivity coupled plasma mass spectrometry（ICP-MS）The running parameter of analysis is as follows：Radio-frequency power 1550W；Sampling
Depth 10mm；Flow rate of carrier gas 1.09Lmin-1；Using He crash modes, 3.4 mLmin of He throughputs-1；Time of integration 2S；
Scan type is single pole.The isotope selected during measure is45Sc, with72Ge is internal standard.
The testing conditions and method that the present invention uses are on the basis of lot of documents is consulted, and explore and grind by many experiments
Study carefully what is screened afterwards, can reach the purpose of accuracy is high, accuracy is high, detection limit is low, stability is good.
The beneficial effects of the invention are as follows：
1st, in a kind of Chinese medicine of the present invention scandium content detection method, expand Chinese medicine heavy metal analysis platform be applicable in
Scope, can better ensure that the quality safety of Chinese medicine, and technological reserve is provided for scandium assay in Chinese medicine.
2nd, in a kind of Chinese medicine of the present invention scandium content detection method, using inductivity coupled plasma mass spectrometry
（ICP-MS）Analyzed, easy to operate, fast and easy, detection efficiency is high, and accuracy is high, and precision is high, and has well
Stability and reappearance.
Embodiment
The present invention is introduced in order to more detailed, with reference to embodiment, the present invention will be further described.Embodiment is simultaneously
It is not the restriction to technical solution of the present invention, it is all based on the modification made in scope of the invention as claimed, still in the present invention
Right in.
Instrument and reagent used be：8800 icp ms of Agilent；Millipore Mill-
Q ultrapure water machines；CEM MARS6 microwave dissolvers；The ML204 types electronic analytical balance (plum Teller-limited public affairs of support benefit instrument
Department).Scandium single element standard solution is purchased from Town in Shanghai spectrum company, producer O2Si, specification 1000mgL-1, lot number 1064277.Citrus
The standard substances such as leaf, spirulina, pollen are purchased from geophysics geochemistry complex investigation institute of Chinese Academy of Geological Sciences.Germanium single element
Titer is purchased from Jinan Zhong Biao Science and Technology Ltd.s, 1000 μ of specificationg·mL-1 , lot number ZBR321；Containing Ce, Co, Li6、Mg、Tl、Y
Tuning solution（1μg·L-1 ）, purchased from Agilent companies.Nitric acid is MERCK top pure grades, and hydrofluoric acid is high-grade pure, and hydrogen peroxide is
Top pure grade, water are the high purity water handled through water purification machine.
Embodiment 1
The detection method of scandium content, comprises the following steps in a kind of Chinese medicine：
（1）The preparation of series standard solution：Precision draws scandium single element titer（1000 mg·L-1）1mL, puts 100m L amounts
In bottle, 2% salpeter solution is added to be diluted to scale, up to scandium standard solution (10mgL-1), then accurate this standard solution of absorption
0.25mL, puts in 10mL measuring bottles, adds 2% salpeter solution to be diluted to scale up to scandium storing solution（0.25 mg·L-1）.Precision is drawn
Scandium storing solution 0.01mL, 0.05 mL, 0.1 mL, 0.5 mL, 1mL, split in 25 mL measuring bottles, add 2% salpeter solution to be diluted to quarter
It is 0.1 μ gL to spend up to scandium concentration-1、0.5μg·L-1、1μg·L-1、5μg·L-1、10μg·L-1Series standard solution.
（2）The preparation of inner mark solution：Precision is drawn germanium standard solution and is put in right amount in measuring bottle, adds 5% salpeter solution to be configured to dense
Spend for 500 μ gL-1Inner mark solution.
（3）The preparation of sample solution：The sample 0.5g for being ground into coarse powder is taken, it is accurately weighed, put in counteracting tank, add 8mL
Nitric acid, 0.5mL hydrofluoric acid, mix and are cleared up in postposition microwave dissolver by certain procedures；Let cool after resolution, put and catch up with acid
On frame 130 DEG C catch up with acid 2.5 it is small when, let cool to room temperature, be transferred in 25ml volumetric flasks, resolution is washed with 2% salpeter solution of volumetric concentration
Tank 3~5 times, is diluted to scale, you can obtain sample solution.
（4）Carry out inductivity coupled plasma mass spectrometry（ICP-MS）Analysis：It is accurate respectively to draw series standard solution and sample
Product solution, injects icp ms, analysis measure is carried out according to certain condition.
（5）Result is calculated：Scandium content is obtained by standard curve.
The micro-wave digestion program is：Using temperature programming, 1030~1800W of power, 20~25min of time-to-climb,
190 DEG C of holding 20min.
The inductivity coupled plasma mass spectrometry（ICP-MS）The running parameter of analysis is as follows：Radio-frequency power 1550W；Sampling
Depth 10mm；Flow rate of carrier gas 1.09Lmin-1；Using He crash modes, 3.4 mLmin of He throughputs-1；Time of integration 2S；
Scan type is single pole.The isotope selected during measure is45Sc, with72Ge is internal standard.
It is as follows that methodology validation experiment is carried out to detection method described in embodiment：
1st, the investigation of solvent species and dosage is cleared up
Using three kinds of Quality Control material citrus leaf, spirulina, pollen with range of uncertainty, resolution solvent is investigated.
Each Quality Control material powder 0.5g is taken, it is accurately weighed, put in counteracting tank, add different resolution solvents, put in microwave dissolver and clear up,
Heated up using Onetouch model programs, time-to-climb：20~25min, keeps 20min after rising to 190 DEG C, and power 1030~
1800W, after let cool, be transferred in 25mL measuring bottles, and be diluted to scale, shaken up with water, sample introduction measure.As a result, simple use
Nitric acid is cleared up, though the measured value of citrus leaf obtains the lowest limit in prescribed limit, close to setting；And use nitric acid hydrogenation fluoric acid
During Acid system, the measured values of three kinds of standard substances therefore determines that resolution solvent adds for 8mL nitric acid close to the intermediate value of specified interval
0.5mL hydrofluoric acid, is shown in Table 1.
The different resolution solvents of table 1 investigate result
2nd, the influence of acid is caught up with
By the preparation method of sample solution of the present invention, sour 2.5h is caught up with 130 DEG C after being respectively compared nitric acid resolution and does not catch up with acid
Influence to scandium measurement result.The result shows that：Catch up with acid to influence measurement result little, be shown in Table 2.It is rotten to instrument to reduce hydrofluoric acid
Erosion, determines to catch up with sour 2.5h at 130 DEG C after Specimen eliminating.
Table 2 catches up with acid to influence to investigate result
3rd, linear relationship is investigated
Series standard solution sample introduction is taken, obtains regression equation：Y=0.0814X+0.0027, R=1.0000, show to work as sample introduction concentration
For 0.1ng/ml~10ng/ml when, it is linear good.
4th, repeatability is investigated
Six parts, every part of 0.5g of citrus leaf is taken, it is accurately weighed, put in counteracting tank, add salpeter solution 8mL, hydrofluoric acid 0.5mL, mix,
Put in microwave dissolver and clear up, let cool, put and catch up with sour frame 130 DEG C when catching up with acid 2.5 small, let cool, 25ml is transferred to 2% salpeter solution
In measuring bottle, and scale is diluted to, shaken up, sample introduction measure.The RSD of six parts of samples is 4.40%, and repeatability meets methodology requirement,
It the results are shown in Table 3.
The repeatability of table 3 investigates result
5th, precision is investigated
Sample solution under repeated item is taken, continuous sample introduction 6 times, the RSD of measured concentration is 0.45%, meets methodology requirement, as a result
It is shown in Table 4.
4 precision of table investigates result
6th, study on the stability
Sample solution under repeated item is taken, the 24 interior measure of sample introduction at regular intervals when small, the RSD of measured concentration is 4.25%, sample
Product are stablized in 24h, the results are shown in Table 5.
5 study on the stability result of table
7th, it is loaded recovery test
Six parts, every part of 0.5g of citrus leaf is taken, it is accurately weighed, put in counteracting tank, precision adds scandium storing solution（0.25 mg·L-1）
0.3mL, by sample-adding solution is prepared under repeated item, sample introduction measure, calculates sample recovery rate, as a result the rate of recovery 90%~
Between 120%, meet trace analysis requirement.
Table 6 is loaded recovery test result
Methodological study the result shows that, the method for the invention can be used for detection Chinese medicine in scandium constituent content.
Claims (3)
1. the detection method of scandium content in a kind of Chinese medicine, it is characterised in that comprise the following steps：
（1）The preparation of series standard solution：Precision draws scandium single element titer（1000 mg·L-1）Add 2% salpeter solution dilute
Release, it is respectively 0.1 μ gL that scandium concentration, which is made,-1、0.5μg·L-1、1μg·L-1、5μg·L-1、10μg·L-1Series standard it is molten
Liquid；
（2）The preparation of inner mark solution：Precision is drawn germanium standard solution and is put in right amount in measuring bottle, adds 5% salpeter solution to be configured to concentration and is
500μg·L-1Inner mark solution；
（3）The preparation of sample solution：Sample 0.4~the 0.8g for being ground into coarse powder is taken, it is accurately weighed, put in counteracting tank, add
Volume ratio is 7~8：0.5~1 nitrate acid and hydrofluoric acid mixed acid, mixes and disappears in postposition microwave dissolver by certain procedures
Solution；Let cool after resolution, put and catch up with sour frame 125~135 DEG C when catching up with acid 2~3 small, let cool to room temperature, be transferred to 25ml volumetric flasks
In, wash counteracting tank 3~5 times with 2% salpeter solution of volumetric concentration, be diluted to scale, you can obtain sample solution；
（4）Carry out inductivity coupled plasma mass spectrometry（ICP-MS）Analysis：Accurate absorption series standard solution and sample are molten respectively
Liquid, injects icp ms, analysis measure is carried out according to certain condition；
（5）Result is calculated：Scandium content is obtained by standard curve.
2. the detection method of scandium content in Chinese medicine according to claim 1, it is characterised in that the micro-wave digestion journey
Sequence is：Using temperature programming, 1030~1800W of power, 20~25min of time-to-climb, 190 DEG C of 20~25min of holding.
3. the detection method of scandium content in Chinese medicine according to claim 1, it is characterised in that described inductive coupling etc. from
Daughter mass spectrum（ICP-MS）The running parameter of analysis is as follows：Radio-frequency power 1550W；Sampling depth 10mm；Flow rate of carrier gas 1.09L
min-1；Using He crash modes, 3.4 mLmin of He throughputs-1；Time of integration 2S；Scan type is single pole；Selected during measure
Fixed isotope is45Sc, with72Ge is internal standard.
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| CN109765288A (en) * | 2019-03-13 | 2019-05-17 | 海检检测有限公司 | A kind of quantitative analysis method of rare earth element Interwell tracer |
| CN110455612A (en) * | 2019-09-08 | 2019-11-15 | 浙江理工大学 | A kind of mulberry leaf and ramulus mori impurity minimizing technology for strontium isotope detection |
| CN110553893A (en) * | 2019-09-08 | 2019-12-10 | 浙江理工大学 | soil impurity removal method for strontium isotope detection |
| CN111505095A (en) * | 2019-10-16 | 2020-08-07 | 中国医学科学院药用植物研究所 | Electrochemical detection method for multiple types of harmful elements in traditional Chinese medicinal materials and preparations thereof |
| CN112683642A (en) * | 2020-12-11 | 2021-04-20 | 无锡福祈制药有限公司 | Method for detecting mercury residual quantity in spiramycin |
| CN112697776A (en) * | 2020-12-11 | 2021-04-23 | 无锡福祈制药有限公司 | Method for detecting residual amounts of Cd, Pd, As, Co, V and Ni in netilmicin sulfate |
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| CN109765288A (en) * | 2019-03-13 | 2019-05-17 | 海检检测有限公司 | A kind of quantitative analysis method of rare earth element Interwell tracer |
| CN110455612A (en) * | 2019-09-08 | 2019-11-15 | 浙江理工大学 | A kind of mulberry leaf and ramulus mori impurity minimizing technology for strontium isotope detection |
| CN110553893A (en) * | 2019-09-08 | 2019-12-10 | 浙江理工大学 | soil impurity removal method for strontium isotope detection |
| CN111505095A (en) * | 2019-10-16 | 2020-08-07 | 中国医学科学院药用植物研究所 | Electrochemical detection method for multiple types of harmful elements in traditional Chinese medicinal materials and preparations thereof |
| CN112683642A (en) * | 2020-12-11 | 2021-04-20 | 无锡福祈制药有限公司 | Method for detecting mercury residual quantity in spiramycin |
| CN112697776A (en) * | 2020-12-11 | 2021-04-23 | 无锡福祈制药有限公司 | Method for detecting residual amounts of Cd, Pd, As, Co, V and Ni in netilmicin sulfate |
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