CN102507721A - Method for measuring antimony in powder cosmetic by microwave digestion and hydrofluoric acid-resistant sampling system ICP-MS (inductively coupled plasma-mass spectrometry) - Google Patents
Method for measuring antimony in powder cosmetic by microwave digestion and hydrofluoric acid-resistant sampling system ICP-MS (inductively coupled plasma-mass spectrometry) Download PDFInfo
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Abstract
The invention relates to a method for detecting the content of antimony in a cosmetic, in particular to a method for measuring the antimony in the powder cosmetic by a microwave digestion and hydrofluoric acid-resistant sampling system ICP-MS (inductively coupled plasma-mass spectrometry). The method comprises the following steps that: after a cosmetic sample is dispelled by nitric acid, hydrogen peroxide and hydrofluoric acid microwaves, organisms are discomposed; sample solution is introduced into an ICP-MS atomizer; high-temperature high-frequency plasmas are loaded by argon to carry out ionization and generate ions; after being focused, the ions enter the spectrometry; characteristic ion abundances of an antimony element and an on-line internal standard rhodium element in the sample solution are detected, wherein the characteristic ion abundance of the antimony element is directly proportional to the content of the antimony element; according to a ratio of an actually measured rhodium internal standard response value to an expected internal standard response value, correcting the response value of the antimony element; carrying out quantitative measurement by adopting an internal standard calibration curve method; calculating the content of the antimony element in the cosmetic; and obtaining the content of the antimony by a conversion factor. The method disclosed by the invention has the characteristics of strong specificity, high sensitivity and accurate result.
Description
Technical field
The present invention relates to the detection method of antimony content in a kind of cosmetics, especially related to the assay method that a kind of employing micro-wave digestion-hydrofluoric acid resistant sampling system inductivity coupled plasma mass spectrometry (ICP-MS) detection technique is measured antimony content in the powder class cosmetics.
Background technology
Along with the upgrading of the level of consumption, China's cosmetics industry keeps average annual rapid growth more than 15%, has become the cosmetics production and marketing big country in Asia second, the world the 7th, and the cosmetics safety problem also more and more causes global attention.In recent years, along with new synthesizing with newfound chemical substance continues to bring out, limit with the growth rate of material kind very fast; But accurately the growth of quantitative detecting method but can not adapt to the growth rate that limits with material, particularly still can not give qualification for limiting with the content of material of from raw material, bringing.Both at home and abroad in Cosmetic Manufacture to limiting use and health of bringing thus and environmental impact with material, become the major issue that concerns people ' s health, social stability even influence international trade relations.China is to the deposit of cosmetic standard detection method; Be only limited at present stipulate in " cosmetics health standard " and GB, the industry standard method less than five, 60 kind; Can not satisfy the needs that cosmetics are imported and exported and domestic production sale safety is checked on far away, more can not satisfy the demand of developing new product and integrating with international cosmetics industry.
Metallic element antimony mainly comes from natural stibnite.B.C. 5000, iron black was used for penciling one's eyebrows and dying eyebrow by the Egyptian.In Ancient Times in China, the compound of antimony also is used as cosmetics and pigment.But ancient times, people's lack of scientific knowledge hardly realized that long-term contact antimony can cause liver, renal damage, can cause blood pressure, rhythm abnormality and skin lesion occurring, caused dry skin, chapped, and eyes and skin are had pungency, dermatitis or eczema occurred.If can cause GI irritation after careless the absorption, feel sick, vomiting, oral cavity and throat burn and central nervous system suppress.Along with the development of industrial automation, the annual consumption of antimony also sharply increases, and bioenvironmental pollution is also caused day by day the extensive concern in the world.In " the cosmetics health standard " 2007 editions of China and European Union's cosmetics instructions (76/768/EEC) all clearly regulation antimony be banned substance.
Through inquiry, the research that at present relevant antimony detects is less, and the domestic current standard does not still have the detection method of antimony in the cosmetics.The domestic document of delivering is very few, these several kinds of main AAS, hydride generation atomic fluorescence method, graphite oven atomic absorption and ICP-AESs.AAS operational processes complex steps, sensitivity is low, stable, reappearance is relatively poor relatively.The method that is applied at present the antimony detection at most is the hydride generation atomic fluorescence method, this method complex operation step, and to current-carrying acidity, reductive agent and hydrogenation conditional request are higher.The graphite oven atomic absorption matrix disturbs very serious, need to add relevant matrix modifier, otherwise sample is measured the no signal value after digesting, and complicated substrate to the graphite-pipe damage greatly, and sensitivity is not high, and reappearance is bad.Also have a small amount of bibliographical information to detect with ICP-AES, this method has advantages such as precision height, matrix effect is little, the range of linearity is wide, but compares with inductively coupled plasma mass spectrometry, and sensitivity and detection limit are relatively poor relatively.The characteristics that inductively coupled plasma mass spectrometry has that detection limit is low, the range of linearity is wide, disturbs less, precision is high can adapt to the mensuration of trace in the complicated substrate or ultratrace element.Powder class cosmetics matrix is formed more complicated; It comprises talcum powder, porcelain earth etc.; Pre-treatment generally adopts wet method to clear up or micro-wave digestion, and then also there is a certain amount of sediment in pre-treatment if not adding hydrofluorite clears up in the digestion solution; Easy absorption antimony such as silicon dioxide in the matrix particularly are to detecting serious interference.Add acid mixture micro-wave digestion samples such as hydrofluorite, the digestion solution clarification is bright, and the testing result recovery is high.But hydrofluorite meeting etching glass instrument accessory, in order to reduce the infringement of hydrofluorite to instrument, this method has adopted the hydrofluoric acid resistant sampling system.At present, do not inquire the bibliographical information that relevant micro-wave digestion-hydrofluoric acid resistant sampling system ICP-MS detection technique is measured antimony content in the cosmetics.
Summary of the invention
The object of the invention is intended to overcome the defective of prior art, and a kind of assay method that adopts micro-wave digestion-hydrofluoric acid resistant sampling system ICP-MS detection technique to measure antimony content in the powder class cosmetics is provided.This method has strong, highly sensitive, the characteristic of accurate as a result of specificity.
In order to realize above-mentioned purpose, the technical scheme below the present invention has adopted:
A kind of micro-wave digestion-hydrofluoric acid resistant sampling system ICP-MS measures the method for antimony in the powder class cosmetics, and this method comprises the steps:
1) take by weighing about 0.5～1.0 g sample, be accurate to 0.001g, mixing places jar in the micro-wave digestion;
2) in the said cosmetic sample of step 1), add 5.0mL nitric acid, the 2.0mL weight percent concentration is 30% hydrogen peroxide, and 2.0mL hydrofluorite makes the abundant submergence of sample, puts microwave digestion system and clears up, and it is following that microwave digestion system is cleared up program:
Step is 1.: power is 1600W, heating-up time 5min, temperature to 120 ℃, retention time 5min;
Step is 2.: power is 1600W, heating-up time 5min, temperature to 180 ℃, retention time 10min;
Step is 3.: power is 1600W, heating-up time 9min, temperature to 200 ℃, retention time 20min;
3) treat counteracting tank cooling after, water repeatedly washes solution in the 25mL plastics volumetric flask on a small quantity, is settled to scale, mixing;
4) preparation standard solution: use 1000 μ g/mL antimony standard inventory solution, using concentration of volume percent is that to become concentration be the antimony standard solution of 0.5,1.0,5.0,10.0,50.0 μ g/L for 1% nitric acid stepwise dilution;
5) draw calibration curve: under the icp ms condition of work of setting; Adopt the hydrofluoric acid resistant sampling system that sample is introduced instrument; And with the online interior mark adding of rhodium standard operation solution; The abundance of ions of antimony element is measured in the positive quantitative analysis method of interior calibration, and interior mark rhodium working concentration is 10 μ g/L; Concentration with antimony element is horizontal ordinate, is ordinate with the abundance of ions of antimony element, instrument computer automatic drafting antimony element calibration curve;
Described icp ms condition of work is following:
Plasma jet: 18L/min,
Assist gas flow: 1.8L/min,
Refrigerating gas flow: 0.14L/min,
Atomization gas flow: 0.90L/min,
Sampling depth: 7.0mm,
Plasma RF power: 1.40kw,
Sample introduction stabilization time: 35s,
Pump speed: 4rpm,
Scan pattern: jump the peak scan pattern,
Scanning times: single-point 30 times,
Multiplicity: 5,
The residence time: 10ms,
Element to be measured and internal standard element isotope:
121Sb,
103Rh,
The hydrofluoric acid resistant sampling system: the atomizer of anti-HF, spray chamber, pipe core are torch pipe, platinum sampling spiroid and the intercepting awl of platinum material;
6) abundance of ions of antimony element and interior mark rhodium element in the sample solution set by step 5) method determination step 3); According to the response that the mark response in the actual measurement rhodium and the ratio of the interior mark of expection response are proofreaied and correct antimony element, use the calibration curve of gained to calculate the antimony element content in the cosmetic sample; The result calculates:
The content of antimony is represented with
in the cosmetics, is calculated as follows:
In the formula:
---the quality of sample, unit is g.
As preferably, the concrete steps of preparation standard solution in the said step 4): accurately draw 0.1mL antimony standard inventory solution, be settled to 100mL, be mixed with the antimony standard and use solution 1 μ g/mL with the salpeter solution of 1% concentration of volume percent; Draw the antimony standard respectively and use solution 0.025mL, 0.050mL, 0.25mL; 0.50mL 2.5mL is settled to the 50mL volumetric flask with the salpeter solution of 1% concentration of volume percent; Mixing, solution concentration is equivalent to every liter 0.5,1.0,5.0,10.0,50.0 μ g standard operation solution in the volumetric flask.
Among the present invention with cosmetic sample behind nitric acid, hydrogen peroxide and hydrofluorite micro-wave digestion, organism is decomposed, and sample solution is imported icp ms (ICP-MS) atomizer; Be written into the high temperature high-frequency plasma by argon gas, ionization takes place, produce ion; Get into mass spectrometer after the ion focus; Antimony element and the online interior characteristic ion abundance of marking rhodium element in the test sample solution, the characteristic ion abundance of antimony element is directly proportional with the content of antimony element, according to surveying mark response and the response of expecting that the interior ratio of marking response is proofreaied and correct antimony element in the rhodium; Calibration directrix curve method is carried out quantitative measurement in adopting, and calculates the content of antimony in the cosmetics.
The present invention has overcome the defective of prior art, has set up that a kind of specificity is strong, highly sensitive, the result is accurate, adopts the method for antimony content in micro-wave digestion-hydrofluoric acid resistant sampling system inductivity coupled plasma mass spectrometry (ICP-MS) technical measurement powder class cosmetics.It is easy, quick, complete that pre-treatment adds nitric acid, hydrogen peroxide, hydrofluorite micro-wave digestion method, overcome the difficult problem of the absorption antimony of silica crystals, and the recovery improves greatly; And component to be measured is pollution not, is difficult for loss, and adopts the ICP-MS spectral line simple; Detecting pattern is flexible, and simple operating steps, accuracy are high, low, the various interference of detection limit is few, detects lower bound and reaches 0.10 mg/kg; The recovery is 85.7%～103%; Relative standard deviation≤5% is enough to satisfy the minimum requirements of the current international practice, is applicable to the detection of cosmetics safety health project.
The present invention has filled up domestic micro-wave digestion-hydrofluoric acid resistant sampling system inductivity coupled plasma mass spectrometry (ICPMS) technology technological gap that antimony detects in cosmetics; Harmful limiting with material detection technique new standard has very significant meaning in the cosmetics for formulating; Healthy to the protection human body simultaneously, promote China's cosmetics industry sound development and foreign trade promotion to have very realistic meanings.
Description of drawings
Fig. 1 is the calibration curve of antimony, and linear equation is y=(7033+13720
x) *
f,
fBe interior calibration positive coefficient, linearly dependent coefficient 0.99998.
Fig. 2 is 1.0 μ g/L Sb
121Standard solution and interior mark 10 μ g/LRh
103Abundance of ions figure.
Embodiment
1. use instrument and instrument condition
1.1 use instrument: icp ms (ICP-MS), model: Bruker 820 MS;
1.2 the atomizer of anti-HF, spray chamber, pipe core are torch pipe, platinum sampling spiroid (diameter 1.1mm), the platinum intercepting awl (diameter 0.5mm) of platinum material;
1.3 the instrument condition of work is seen table 1
The operating condition reference of table 1. instrument
| Project | Running parameter |
| Plasma jet | 18 L/min |
| The assist gas flow | 1.8 L/min |
| The refrigerating gas flow | 0.14 L/min |
| The atomization gas flow | 0.90 L/min |
| Sampling depth | 7.0 mm |
| Plasma RF power | 1.40 kw |
| Sample introduction stabilization time | 35 s |
| Pump speed | 4 rpm |
| Scan pattern | Jump the peak scan pattern |
| Scanning times | Single- |
| Multiplicity | 5 |
| The |
10 ms |
| Element to be measured and internal standard element isotope | 121Sb， 103Rh |
| The hydrofluoric acid resistant sampling system | The atomizer of anti-HF, spray chamber, pipe core are torch pipe, platinum sampling spiroid and the intercepting awl of platinum material |
2. use reagent:
2.1 it is pure that agents useful for same is top grade, experimental water is the one-level water that meets regulation among the GB/T 6682;
2.2 nitric acid (ρ 1.42g/mL); Hydrogen peroxide (the 30% percentage by weight WS); Hydrofluorite (the 40% percentage by weight WS);
2.3 antimony standard inventory solution: with national standard reagent (GBW), concentration is 1000 μ g/mL;
2.4 rhodium standard inventory solution: with national standard reagent (GBW), concentration is 1000 μ g/mL;
2.5 stock solution (10 μ g/mL) in the middle of the antimony standard: draw 1.0 mL antimony standard inventory solution (2.4), (1+99) is settled to 100 mL with salpeter solution;
2.6 antimony standard operation liquid: the middle stock solution (2.5) of the 1.0 mL antimony standards of accurately drawing, (1+99) is settled to 10 mL with salpeter solution.
3. Specimen eliminating
Take by weighing about 0.5g sample (being accurate to 0.001 g), place jar in the micro-wave digestion, add 5.0 mL nitric acid (look the decision of Specimen eliminating complexity and whether need soak placement), and then add hydrogen peroxide 2.0 mL, hydrofluorite 2.0 mL make the abundant submergence of sample.Put microwave digestion system and clear up, clear up program and see table 2.After treating the counteracting tank cooling, water repeatedly washes solution in the 25 mL volumetric flasks on a small quantity, is settled to scale, mixing.
Table 2 micro-wave digestion device is cleared up program
| Step | Power (W) | Heating-up time (min) | Temperature (℃) | Retention time (min) |
| |
1600 | 5 | 120 | 5 |
| |
1600 | 5 | 180 | 10 |
| |
1600 | 9 | 200 | 20 |
4. calibration curve is drawn
The 1 μ g/mL antimony standard of drawing is respectively used solution 0.025 mL, 0.050 mL, 0.25 mL; 0.50 mL, 2.5 mL are settled to 50 mL volumetric flasks with (1+99) salpeter solution; Mixing is mixed with 0.5,1.0,5.0,10 .0,50.0 μ g/L standard operation solution.
Series standard solution imported in the instrument atomization system transfer to top condition measure.Concentration with antimony element is horizontal ordinate, is ordinate with the abundance of ions of antimony element, instrument computer automatic drafting typical curve.
5. sample determination
Under table 1 condition, with measuring in sample solution and the reagent blank liquid importing hydrofluoric acid resistant sampling system.The intensity rate and the working curve of antimony element and internal standard element are relatively obtained the antimony element content in the cosmetic sample.Converse the content of antimony in the cosmetics again through computing formula as a result.
The result calculates:
The content of antimony is represented with
in the cosmetics, calculates by formula (1):
In the formula:
---the quality of sample; Unit is gram, g.
Result of calculation keeps three position effective digitals.
Antimony detection lower bound is 0.10 mg/kg in the cosmetics of the present invention; Through powder class cosmetic sample recovery of standard addition is tested, the recovery is 85.7%～103%, relative standard deviation≤5%; Meet the requirement of GB/T 27404-2008, prove the feasibility of above-mentioned detection method.The inventive method satisfies the minimum requirements of the current international practice, is applicable to the detection of cosmetics safety health project.
Claims (2)
1. a micro-wave digestion-hydrofluoric acid resistant sampling system ICP-MS measures the method for antimony in the powder class cosmetics, it is characterized in that this method comprises the steps:
1) take by weighing about 0.5 g sample, be accurate to 0.001g, mixing places jar in the micro-wave digestion;
2) in the said cosmetic sample of step 1), add 5.0mL nitric acid, the 2.0mL weight percent concentration is 30% hydrogen peroxide, and 2.0mL hydrofluorite makes the abundant submergence of sample, puts microwave digestion system and clears up, and it is following that microwave digestion system is cleared up program:
Step is 1.: power is 1600W, heating-up time 5min, temperature to 120 ℃, retention time 5min;
Step is 2.: power is 1600W, heating-up time 5min, temperature to 180 ℃, retention time 10min;
Step is 3.: power is 1600W, heating-up time 9min, temperature to 200 ℃, retention time 20min;
3) treat counteracting tank cooling after, water repeatedly washes solution in the 25mL plastics volumetric flask on a small quantity, is settled to scale, mixing;
4) preparation standard solution: use 1000 μ g/mL antimony standard inventory solution, using concentration of volume percent is that to become concentration be the antimony standard solution of 0.5,1.0,5.0,10.0,50.0 μ g/L for 1% nitric acid stepwise dilution;
5) draw calibration curve: under the icp ms condition of work of setting; Adopt the hydrofluoric acid resistant sampling system that sample is introduced instrument; And with the online interior mark adding of rhodium standard operation solution; The abundance of ions of antimony element is measured in the positive quantitative analysis method of interior calibration, and mark use liquid concentration is 10 μ g/L in the rhodium; Concentration with antimony element is horizontal ordinate, is ordinate with the abundance of ions of antimony element, instrument computer automatic drafting antimony element calibration curve;
Described icp ms condition of work is following:
Plasma jet: 18L/min,
Assist gas flow: 1.8L/min,
Refrigerating gas flow: 0.14L/min,
Atomization gas flow: 0.90L/min,
Sampling depth: 7.0mm,
Plasma RF power: 1.40kw,
Sample introduction stabilization time: 35s,
Pump speed: 4rpm,
Scan pattern: jump the peak scan pattern,
Scanning times: single-point 30 times,
Multiplicity: 5,
The residence time: 10ms,
Element to be measured and internal standard element isotope:
121Sb,
103Rh,
The hydrofluoric acid resistant sampling system: the atomizer of anti-HF, spray chamber, pipe core are torch pipe, platinum sampling spiroid and the intercepting awl of platinum material;
6) abundance of ions of antimony element and interior mark rhodium element in the sample solution set by step 5) method determination step 3); The response that root is proofreaied and correct antimony element according to the mark response in the actual measurement rhodium and the ratio of the interior mark of expection response uses the calibration curve of gained to calculate the antimony element content in the cosmetic sample; The content of antimony is represented with
in the cosmetics, is calculated as follows:
In the formula:
---the concentration of tested element in the sample solution, unit is μ g/L;
---sample solution constant volume, unit are mL;
---the quality of sample, unit is g.
2.
a kind of micro-wave digestion according to claim 1-hydrofluoric acid resistant sampling system ICP-MS measures the method for antimony in the powder class cosmetics; The concrete steps that it is characterized in that preparation standard solution in the said step 4): accurately draw 0.1mL antimony standard inventory solution; Be settled to 100mL with 1% concentration of volume percent salpeter solution, be mixed with the antimony standard and use solution 1 μ g/mL; Draw the antimony standard respectively and use solution 0.025mL, 0.050mL, 0.25mL; 0.50mL 2.5mL is settled to the 50mL volumetric flask with 1% concentration of volume percent salpeter solution; Mixing, solution concentration is equivalent to every liter 0.5,1.0,5.0,10.0,50.0 μ g standard operation solution in the volumetric flask.
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| CN103234955A (en) * | 2013-04-24 | 2013-08-07 | 天津虹炎科技有限公司 | Method for measuring antimony metal in powder sample |
| CN104698071A (en) * | 2015-03-20 | 2015-06-10 | 浙江中烟工业有限责任公司 | Method for determining potassium content in cigarette paper |
| CN104698065A (en) * | 2015-03-20 | 2015-06-10 | 浙江中烟工业有限责任公司 | Method for simultaneously measuring sodium content and magnesium content in cigarette paper |
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| CN106404515A (en) * | 2016-11-08 | 2017-02-15 | 苏州恒润商品检验有限公司 | Detection method for determining multiple elements in solid cosmetic powder |
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| CN112763481A (en) * | 2021-01-26 | 2021-05-07 | 山西太钢不锈钢股份有限公司 | Method for measuring trace selenium, cerium, zirconium, tantalum and tellurium content in nickel-based alloy by ICP-MS method |
| CN112763481B (en) * | 2021-01-26 | 2023-12-29 | 山西太钢不锈钢股份有限公司 | Method for measuring trace selenium, cerium, zirconium, tantalum and tellurium content in nickel-based alloy by ICP-MS method |
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