CN107991376A - The method of 5 kinds of element synchronization detections in Gegen Qinlian preparation - Google Patents
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Abstract
The invention discloses the method for 5 kinds of element synchronization detections in Gegen Qinlian preparation, analyzed using inductively coupled plasma mass spectrometry, its detecting step includes：（1）Prepare calibration curve solution；（2）Prepare inner mark solution；（3）Prepare 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.It can better ensure that the quality safety of Gegen Qinlian preparation, the measure for 5 kinds of copper in Gegen Qinlian preparation, arsenic, cadmium, lead and mercury elements provides technological reserve.
Description
Technical field
The present invention relates to medicine detection field, is specifically the method that 5 kinds of element synchronizations detect in Gegen Qinlian preparation.
Background technology
Gegen Qinlian preparation, including Gegen Qinlian Tablets, Gegen Qinlian ball and GEGEN QINLIAN DIWAN etc..For heat-clearing formula, have
The effect of expelling pathogenic factors from muscles for clearing heat, antidiarrheal stop dysentery, cure mainly dysentery, the hot polydipsia of body, diarrhea is smelly dirty；Bacillary dysentery, enteritis.《Chinese Pharmacopoeia》
In versions in 2010, Gegen Qinlian Tablets and Gegen Qinlian ball（Pellet）Prescription it is consistent, by pueraria lobata, radix scutellariae, the coptis, honey-fried licorice root etc.
Four traditional Chinese medicine forms：Pueraria lobata 1000g, radix scutellariae 375g, coptis 375g, honey-fried licorice root 250g.
In recent years, subject great pressure with the high speed development of China's economic, the ecological environment in China.Industrialization
The pollution of the soil, air, water source that bring causes the growing environment of Chinese medicine very important influence.As traditional Chinese medicine is in state
Increasingly it is taken seriously on border, the exogenous pollution of Chinese medicine becomes all circles' focus of attention.Various countries are residual to pollutant in Chinese medicine
The limitation regulation stayed, becomes the big technical barrier that Chinese medicine is gone abroad.To understand the content distribution of each element in the kind, greatly
The residual condition of poisonous and harmful element in the commercially available Gegen Qinlian preparation of grasp is caused, using ICP-MS measure Gegen Qinlian Tablets, pueraria lobata
A kind of reed mentioned in ancient books connects ball（Pellet）In lead, cadmium, arsenic, mercury, the content of copper.
The content of the invention
The purpose of the present invention is to expand the scope of application of Chinese medicine Element detection platform, ensure the quality peace of Chinese medicine
Entirely, there is provided the method for 5 kinds of element synchronization detections in Gegen Qinlian preparation.
The present invention is achieved through the following technical solutions：
The method of 5 kinds of element synchronization detections, 5 kinds of elements are in Gegen Qinlian preparation：Copper, arsenic, cadmium, lead, mercury；Its detection side
Method comprises the following steps：
（1）Prepare calibration curve solution；
（2）Prepare inner mark solution：Accurate germanium, indium, the indium single element standard solution drawn is placed in volumetric flask respectively, molten with 5% nitric acid
Liquid dilutes, and the mixing inner mark solution that germanium, indium, bismuth three constituent content are 200ng/mL is made；
（3）Prepare sample solution：Take Gegen Qinlian formulation samples to grind, take 0.4g, it is accurately weighed, put in counteracting tank, add nitre
Sour 7.0ml, puts in microwave dissolver, is cleared up by certain resolution program.After resolution, counteracting tank is set to naturally cool to room
Temperature, is transferred in 50ml colorimetric cylinders with water, and is diluted to scale, takes 7ml solution to cross 0.45 μm of miillpore filter, it is molten to obtain sample
Liquid；Reagent blank is done in retinue；
（4）Carry out inductivity coupled plasma mass spectrometry（ICP-MS）Analysis：It is accurate respectively to draw standard solution and sample solution, note
Enter icp ms, be detected according to certain condition；
（5）Result is calculated：The content of 5 kinds of elements is obtained by standard curve.
The preparation of the standard solution, including copper, arsenic, cadmium, the preparation of four element mixed standard solution of lead and mercury standard are bent
The preparation of line；The standard curve range of linearity concentration of each element is：Copper（Cu）10~100 μ g/L；Arsenic（As）1~100 μ g/L；
Cadmium（Cd）0.1~10 μ g/L；Lead（Pb）1~100 μ g/L；Mercury（Hg）0.1~2 μ g/L.
The resolution program is as follows：
The inductivity coupled plasma mass spectrometry（ICP-MS）The running parameter of analysis is as follows：Nebulizer pressure 1.8bar；ICP is just
To power；Reflection power 4W；Sample lifts time 40s.
The preparation of the copper, arsenic, cadmium, four element blended standard curve solution of lead, its preparation method include：
（1）Precision draws copper single element standard solution（1000 μg/mL）1ml, arsenic single element standard solution（1000 μg/mL）
1ml, cadmium single element standard solution（1000 μg/mL）0.1ml, lead single element standard solution（1000 μg/mL）1ml, splits not
In same 100mL measuring bottles, scale is diluted to 5% salpeter solution, it is respectively 10 μ g/mL, cadmium content that copper, arsenic, lead content, which is made,
For the standard reserving solution of 1 μ g/mL.
（2）Mixed mark 1：It is accurate respectively to draw 0. 1ml of copper storing solution, arsenic storing solution 0.01ml, cadmium storing solution 0.01ml, lead
Storing solution 0.01ml, puts in same 100ml measuring bottles, and scale is diluted to 5% salpeter solution, and copper content is made as 10ng/ml, arsenic
The mixed standard solution that content is 1ng/ml, cadmium content 0.1ng/ml, lead content are 1ng/ml.
（3）Mixed mark 2：It is accurate respectively to draw 0. 2ml of copper storing solution, arsenic storing solution 0.1ml, cadmium storing solution 0.1ml, lead storage
Standby liquid 0.1ml, puts in same 100ml measuring bottles, scale is diluted to 5% salpeter solution, and copper content is made and contains for 20 ng/ml, arsenic
Measure as 10 ng/ml, cadmium content are 1 ng/ml, lead content is 10ng/ml mixed standard solution.
（4）Mixed mark 3：It is accurate respectively to draw 0. 5ml of copper storing solution, arsenic storing solution 0.5ml, cadmium storing solution 0.5ml, lead storage
Standby liquid 0.5ml, puts in same 100ml measuring bottles, scale is diluted to 5% salpeter solution, and copper content is made and contains for 50 ng/ml, arsenic
Measure as 50 ng/ml, cadmium content are 5 ng/ml, lead content is 50 ng/ml mixed standard solution.
（5）Mixed mark 4：It is accurate respectively to draw 0. 8ml of copper storing solution, arsenic storing solution 0.8ml, cadmium storing solution 0.8ml, lead storage
Standby liquid 0.8ml, puts in same 100ml measuring bottles, scale is diluted to 5% salpeter solution, and copper content is made and contains for 80 ng/ml, arsenic
Measure as 80 ng/ml, cadmium content are 8 ng/ml, lead content is 80 ng/ml mixed standard solution.
（6）Mixed mark 5：It is accurate respectively to draw copper storing solution 1ml, arsenic storing solution 1ml, cadmium storing solution 1ml, lead storing solution 1ml,
Put in same 100ml measuring bottles, scale be diluted to 5% salpeter solution, be made copper content be 100 ng/ml, arsenic content be 100
The mixed standard solution that ng/ml, cadmium content are 10 ng/ml, lead content is 100 ng/ml.
The preparation of the mercury calibration curve solution, its preparation method include：
（1）Precision draws mercury single element standard solution（1000 μg/mL）0.1ml, puts in 100mL measuring bottles, dilute with 5% salpeter solution
Release to scale, the mercurous standard solution for being 1 μ g/mL is made, precision is drawn this standard solution 1ml, put in 10ml measuring bottles, with 5%
Salpeter solution is diluted to scale, obtains the storing solution that mercury concentration is 100 ng/mL.
（2）It is accurate respectively to draw mercury standard reserving solution 0.05ml, 0.25ml, 0.5ml, 0.75ml, 1ml, split five
In 50ml volumetric flasks, scale is diluted to 5% salpeter solution, be made mercury content for 0.1 ng/mL, 0.5 ng/mL, 1 ng/mL,
The series standard solution of 1.5 ng/mL, 2 ng/mL.
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, the method that 5 kinds of element synchronizations detect in Gegen Qinlian preparation of the present invention, can better ensure that Gegen Qinlian system
The quality safety of agent, the measure for harmful elements such as copper, arsenic, cadmium, lead and mercury in Gegen Qinlian preparation provide technological reserve；May be used also
To provide important reference frame for the foundation of company standard.
2nd, the method that 5 kinds of element synchronizations detect in Gegen Qinlian preparation of the present invention, easy to operate, fast and easy, inspection
Survey efficient；Using inductivity coupled plasma mass spectrometry（ICP-MS）To be analyzed, accuracy is high, and precision is high, and with good
Good stability and reappearance.
3rd, in Gegen Qinlian preparation of the present invention in the method for 5 kinds of element synchronization detections, when preparing standard curve, including
Copper, arsenic, cadmium, the preparation of four element mixed standard solution of lead and the preparation of mercury standard curve, greatly reduce the use of solution
Amount, and standard curve stock solution is once prepared and is used multiple times, and is improved work efficiency；The preparation of sample solution uses microwave
The mode of resolution, is added nitric acid as digestion agent, Specimen eliminating can be made complete, and can be prepared together with multiple samples.
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：Mars6 microwave dissolvers（CEM companies）, Agilent ICP-MS 7700X,
Merck nitric acid, ultra-pure water（Prepared by MILLIPORE ultrapure water systems）.Copper, arsenic, cadmium, lead, mercury, germanium, bismuth, indium single element standard
Solution is purchased from State center for standard matter.Gegen Qinlian Tablets, Gegen Qinlian ball（Pellet）It is state's sample drawing in 2013, wherein Pueraria lobota
Root a kind of reed mentioned in ancient books connects pellet（Pellet）For exclusive kind.
Embodiment 1
The method of 5 kinds of element synchronization detections, 5 kinds of elements are in Gegen Qinlian preparation：Copper, arsenic, cadmium, lead, mercury；Its detection side
Method is implemented using following technical scheme：
（1）Prepare calibration curve solution；
（2）Prepare inner mark solution：Accurate germanium, indium, the indium single element standard solution drawn is placed in volumetric flask respectively, molten with 5% nitric acid
Liquid dilutes, and the mixing inner mark solution that germanium, indium, bismuth three constituent content are 200ng/mL is made；
（3）Prepare sample solution：Take Gegen Qinlian formulation samples to grind, take 0.4g, it is accurately weighed, put in counteracting tank, add nitre
Sour 7.0ml, puts in microwave dissolver, is cleared up by certain resolution program.After resolution, counteracting tank is set to naturally cool to room
Temperature, is transferred in 50ml colorimetric cylinders with water, and is diluted to scale, takes 7ml solution to cross 0.45 μm of miillpore filter, it is molten to obtain sample
Liquid；Reagent blank is done in retinue；
（4）Carry out inductivity coupled plasma mass spectrometry（ICP-MS）Analysis：It is accurate respectively to draw standard solution and sample solution, note
Enter icp ms, be detected according to certain condition；
（5）Result is calculated：The content of 5 kinds of elements is obtained by standard curve.
The preparation of the standard solution, including copper, arsenic, cadmium, the preparation of four element mixed standard solution of lead and mercury standard are bent
The preparation of line；The standard curve range of linearity concentration of each element is：Copper（Cu）10~100 μ g/L；Arsenic（As）1~100 μ g/L；
Cadmium（Cd）0.1~10 μ g/L；Lead（Pb）1~100 μ g/L；Mercury（Hg）0.1~2 μ g/L.
The resolution program is as follows：
The inductivity coupled plasma mass spectrometry（ICP-MS）The running parameter of analysis is as follows：Nebulizer pressure 1.8bar；ICP is just
To power；Reflection power 4W；Sample lifts time 40s.
The preparation of the copper, arsenic, cadmium, four element blended standard curve solution of lead, its preparation method include：
（1）Precision draws copper single element standard solution（1000 μg/mL）1ml, arsenic single element standard solution（1000 μg/mL）
1ml, cadmium single element standard solution（1000 μg/mL）0.1ml, lead single element standard solution（1000 μg/mL）1ml, splits not
In same 100mL measuring bottles, scale is diluted to 5% salpeter solution, it is respectively 10 μ g/mL, cadmium content that copper, arsenic, lead content, which is made,
For the standard reserving solution of 1 μ g/mL.
（2）Mixed mark 1：It is accurate respectively to draw 0. 1ml of copper storing solution, arsenic storing solution 0.01ml, cadmium storing solution 0.01ml, lead
Storing solution 0.01ml, puts in same 100ml measuring bottles, and scale is diluted to 5% salpeter solution, and copper content is made as 10ng/ml, arsenic
The mixed standard solution that content is 1ng/ml, cadmium content 0.1ng/ml, lead content are 1ng/ml.
（3）Mixed mark 2：It is accurate respectively to draw 0. 2ml of copper storing solution, arsenic storing solution 0.1ml, cadmium storing solution 0.1ml, lead storage
Standby liquid 0.1ml, puts in same 100ml measuring bottles, scale is diluted to 5% salpeter solution, and copper content is made and contains for 20 ng/ml, arsenic
Measure as 10 ng/ml, cadmium content are 1 ng/ml, lead content is 10ng/ml mixed standard solution.
（4）Mixed mark 3：It is accurate respectively to draw 0. 5ml of copper storing solution, arsenic storing solution 0.5ml, cadmium storing solution 0.5ml, lead storage
Standby liquid 0.5ml, puts in same 100ml measuring bottles, scale is diluted to 5% salpeter solution, and copper content is made and contains for 50 ng/ml, arsenic
Measure as 50 ng/ml, cadmium content are 5 ng/ml, lead content is 50 ng/ml mixed standard solution.
（5）Mixed mark 4：It is accurate respectively to draw 0. 8ml of copper storing solution, arsenic storing solution 0.8ml, cadmium storing solution 0.8ml, lead storage
Standby liquid 0.8ml, puts in same 100ml measuring bottles, scale is diluted to 5% salpeter solution, and copper content is made and contains for 80 ng/ml, arsenic
Measure as 80 ng/ml, cadmium content are 8 ng/ml, lead content is 80 ng/ml mixed standard solution.
（6）Mixed mark 5：It is accurate respectively to draw copper storing solution 1ml, arsenic storing solution 1ml, cadmium storing solution 1ml, lead storing solution 1ml,
Put in same 100ml measuring bottles, scale be diluted to 5% salpeter solution, be made copper content be 100 ng/ml, arsenic content be 100
The mixed standard solution that ng/ml, cadmium content are 10 ng/ml, lead content is 100 ng/ml.
The preparation of the mercury calibration curve solution, its preparation method include：
（1）Precision draws mercury single element standard solution（1000 μg/mL）0.1ml, puts in 100mL measuring bottles, dilute with 5% salpeter solution
Release to scale, the mercurous standard solution for being 1 μ g/mL is made, precision is drawn this standard solution 1ml, put in 10ml measuring bottles, with 5%
Salpeter solution is diluted to scale, obtains the storing solution that mercury concentration is 100 ng/mL.
（2）It is accurate respectively to draw mercury standard reserving solution 0.05ml, 0.25ml, 0.5ml, 0.75ml, 1ml, split five
In 50ml volumetric flasks, scale is diluted to 5% salpeter solution, be made mercury content for 0.1 ng/mL, 0.5 ng/mL, 1 ng/mL,
The series standard solution of 1.5 ng/mL, 2 ng/mL.
In determination sample, there is the standard substance of card as quality control reference substance using country, surveyed at the same time together with sample
The content of 5 kinds of elements more than fixed, the quality control traced to the source as measured value, as shown in table 1.
Table 1 analyzes the verification of quality
Case 1
According to the detection method described in above-described embodiment, 19 batches of Gegen Qinlian formulation samples progress copper that different enterprises are produced,
Arsenic, cadmium, the measure of 5 kinds of elements of lead and mercury, measurement result are as shown in table 2.
The determination data of 2 19 batches of samples of table
Claims (6)
1. the method for 5 kinds of element synchronizations detection in Gegen Qinlian preparation, it is characterised in that 5 kinds of elements are：Copper, arsenic, cadmium,
Lead, mercury；Its detection method comprises the following steps：
（1）Prepare calibration curve solution；
（2）Prepare inner mark solution：Accurate germanium, indium, the indium single element standard solution drawn is placed in volumetric flask respectively, molten with 5% nitric acid
Liquid dilutes, and the mixing inner mark solution that germanium, indium, bismuth three constituent content are 200ng/mL is made；
（3）Prepare sample solution：Take Gegen Qinlian formulation samples to grind, take 0.4g, it is accurately weighed, put in counteracting tank, add nitre
Sour 7.0ml, puts in microwave dissolver, is cleared up by certain resolution program；After resolution, counteracting tank is set to naturally cool to room
Temperature, is transferred in 50ml colorimetric cylinders with water, and is diluted to scale, takes 7ml solution to cross 0.45 μm of miillpore filter, it is molten to obtain sample
Liquid；Reagent blank is done in retinue；
（4）Carry out inductivity coupled plasma mass spectrometry（ICP-MS）Analysis：It is accurate respectively to draw standard solution and sample solution, note
Enter icp ms, be detected according to certain condition；
（5）Result is calculated：The content of 5 kinds of elements is obtained by standard curve.
2. the method for 5 kinds of element synchronization detections in Gegen Qinlian preparation according to claim 1, it is characterised in that described
The preparation of standard solution, including copper, arsenic, cadmium, the preparation of four element mixed standard solution of lead and the preparation of mercury standard curve；Each member
Element standard curve range of linearity concentration be：Copper（Cu）10~100 μ g/L；Arsenic（As）1~100 μ g/L；Cadmium（Cd）0.1~10
μg/L；Lead（Pb）1~100 μ g/L；Mercury（Hg）0.1~2 μ g/L.
3. the method for 5 kinds of element synchronization detections in Gegen Qinlian preparation according to claim 1, it is characterised in that described
Resolution program it is as follows.
4. the method for 5 kinds of element synchronization detections in Gegen Qinlian preparation according to claim 1, it is characterised in that described
Inductivity coupled plasma mass spectrometry（ICP-MS）The running parameter of analysis is as follows：Nebulizer pressure 1.8bar；ICP forward powers；
Reflection power 4W；Sample lifts time 40s.
5. the preparation of copper, arsenic, cadmium, four element blended standard curve solution of lead according to claim 2, it is characterised in that its
Preparation method includes：
（1）Precision draws copper single element standard solution（1000 μg/mL）1ml, arsenic single element standard solution（1000 μg/mL）
1ml, cadmium single element standard solution（1000 μg/mL）0.1ml, lead single element standard solution（1000 μg/mL）1ml, splits not
In same 100mL measuring bottles, scale is diluted to 5% salpeter solution, it is respectively 10 μ g/mL, cadmium content that copper, arsenic, lead content, which is made,
For the standard reserving solution of 1 μ g/mL；
（2）Mixed mark 1：It is accurate respectively to draw 0. 1ml of copper storing solution, arsenic storing solution 0.01ml, cadmium storing solution 0.01ml, lead deposit
Liquid 0.01ml, puts in same 100ml measuring bottles, and scale is diluted to 5% salpeter solution, and copper content is made as 10ng/ml, arsenic content
The mixed standard solution for being 1ng/ml for 1ng/ml, cadmium content 0.1ng/ml, lead content；
（3）Mixed mark 2：It is accurate respectively to draw 0. 2ml of copper storing solution, arsenic storing solution 0.1ml, cadmium storing solution 0.1ml, lead storing solution
0.1ml, puts in same 100ml measuring bottles, and scale is diluted to 5% salpeter solution, be made copper content be 20 ng/ml, arsenic content be
The mixed standard solution that 10 ng/ml, cadmium content are 1 ng/ml, lead content is 10ng/ml；
（4）Mixed mark 3：It is accurate respectively to draw 0. 5ml of copper storing solution, arsenic storing solution 0.5ml, cadmium storing solution 0.5ml, lead storing solution
0.5ml, puts in same 100ml measuring bottles, and scale is diluted to 5% salpeter solution, be made copper content be 50 ng/ml, arsenic content be
The mixed standard solution that 50 ng/ml, cadmium content are 5 ng/ml, lead content is 50 ng/ml；
（5）Mixed mark 4：It is accurate respectively to draw 0. 8ml of copper storing solution, arsenic storing solution 0.8ml, cadmium storing solution 0.8ml, lead storing solution
0.8ml, puts in same 100ml measuring bottles, and scale is diluted to 5% salpeter solution, be made copper content be 80 ng/ml, arsenic content be
The mixed standard solution that 80 ng/ml, cadmium content are 8 ng/ml, lead content is 80 ng/ml；
（6）Mixed mark 5：It is accurate respectively to draw copper storing solution 1ml, arsenic storing solution 1ml, cadmium storing solution 1ml, lead storing solution 1ml, put same
In one 100ml measuring bottles, scale is diluted to 5% salpeter solution, be made copper content be 100 ng/ml, arsenic content be 100 ng/ml,
The mixed standard solution that cadmium content is 10 ng/ml, lead content is 100 ng/ml.
6. the preparation of mercury calibration curve solution according to claim 2, it is characterised in that its preparation method includes：
（1）Precision draws mercury single element standard solution（1000 μg/mL）0.1ml, puts in 100mL measuring bottles, dilute with 5% salpeter solution
Release to scale, the mercurous standard solution for being 1 μ g/mL is made, precision is drawn this standard solution 1ml, put in 10ml measuring bottles, with 5%
Salpeter solution is diluted to scale, obtains the storing solution that mercury concentration is 100 ng/mL；
（2）It is accurate respectively to draw mercury standard reserving solution 0.05ml, 0.25ml, 0.5ml, 0.75ml, 1ml, split five 50ml and hold
In measuring bottle, scale is diluted to 5% salpeter solution, mercury content is made as 0.1 ng/mL, 0.5 ng/mL, 1 ng/mL, 1.5 ng/
The series standard solution of mL, 2 ng/mL.
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| CN116593568A (en) * | 2023-05-16 | 2023-08-15 | 山东省疾病预防控制中心 | Method for simultaneously detecting contents of multiple heavy metals in Chinese herbal medicine and application |
| CN116593568B (en) * | 2023-05-16 | 2024-05-10 | 山东省疾病预防控制中心 | Method for simultaneously detecting contents of multiple heavy metals in Chinese herbal medicine and application |
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Application publication date: 20180504 |