Method for detecting migration quantity of nine metals in cosmetic packaging material and application of method
By using ICP-MS to detect the migration levels of nine metals in cosmetic packaging materials, the problem of inconsistent testing standards in existing technologies has been solved, enabling efficient and accurate detection and risk assessment of heavy metal migration levels.
Patent Information
- Application Number
- CN202511948411.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-23
- Publication Date
- 2026-03-27
AI Technical Summary
There is a lack of systematic and unified standards for detecting the migration of heavy metals in existing cosmetic packaging materials. In particular, there is a gap in the simultaneous detection of nine potentially harmful elements, including chromium, cobalt, nickel, selenium, strontium, zirconium, antimony, barium, and thallium. Furthermore, there is a lack of simulated migration test protocols and sample pretreatment methods, which leads to inaccurate risk assessments.
Inductively coupled plasma mass spectrometry (ICP-MS) was used for detection. By designing different pretreatment methods for soaking solutions, sample migration experiments were conducted on cosmetic simulation solutions containing acid, alcohol, and oil. Standard solutions were prepared for quantitative analysis by combining steps such as membrane filtration, heating digestion, and microwave digestion.
It enables simultaneous detection of nine metals, improving detection efficiency and accuracy, meeting safety regulatory requirements, and is suitable for risk assessment of heavy metal migration in cosmetic packaging materials.
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Figure CN121740994A_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The application belongs to the field of detection, and particularly relates to a method for detecting migration amounts of nine metals in cosmetic package materials and application thereof. BACKGROUND
[0002] The existing safety evaluation of cosmetic package materials lacks a systematic and unified detection standard for heavy metal migration amounts, especially the synchronous detection of nine potentially harmful elements such as chromium, cobalt, nickel, selenium, strontium, zirconium, antimony, barium and thallium. The lack of simulation migration test schemes and sample pretreatment methods for the interaction between different components of cosmetics and package materials leads to inaccurate risk assessment. The application performs migration experiments by analyzing the components of the selected blank simulation liquid close to the cosmetics, uses different pretreatment methods for different soaking liquids, and uses an inductively coupled plasma mass spectrometer for determination, qualitative analysis by element-specific mass number, and quantitative analysis by external standard method.
[0003] In the research on investigation and research on heavy metal detection methods in cosmetics by Tan Jingrong, Liu Wei, Zhang Yiting, Li Xue, etc., three methods for detecting heavy metals in cosmetics are proposed, including instrument analysis method, electrochemical method and chemical colorimetry. However, the pre-sequence treatment of different types of cosmetics is not further studied in this paper. On the basis of general detection, the pre-sequence treatment and migration steps of different cosmetics are supplemented, providing a new method for package material detection. SUMMARY
[0004] In view of the problems existing in the prior art, the purpose of the application is to design a method for detecting migration amounts of nine metals in cosmetic package materials and application thereof.
[0005] The application specifically adopts the following technical solutions to achieve the above purpose: The first aspect of the application provides a method for detecting migration amounts of nine metals in cosmetic package materials, which comprises the following steps: (S.1) Sample acquisition: take cosmetic simulation liquid, which is divided into acid-containing cosmetic simulation liquid, alcohol-containing cosmetic simulation liquid and oil-containing cosmetic simulation liquid; (S.2) Sample migration: fill the cosmetic simulation liquid into the cosmetic package material to be tested, seal, and heat the sealed package material; (S.3) Sample pretreatment: take the cosmetic simulation liquid in the package material and perform the following treatment, the acid-containing cosmetic simulation liquid is filtered through a filter membrane; the alcohol-containing cosmetic simulation liquid is heated to near dryness, diluted with nitric acid, and filtered; the oil-containing cosmetic simulation liquid is added with nitric acid, heated for pre-digestion, cooled to room temperature after pre-digestion, subjected to microwave digestion, heated to not emit yellow smoke after digestion, diluted with deionized water, and filtered; (S.4) Test by ICP-MS instrument, collect and process data; (S.5) Prepare standard solution, calculate the content of each element.
[0006] Further, the 9 metals include chromium, cobalt, nickel, selenium, strontium, zirconium, antimony, barium and thallium.
[0007] Further, the acid-containing cosmetic simulation solution is 4% acetic acid, the alcohol-containing cosmetic simulation solution is 10%-90% ethanol, and the oil-containing cosmetic simulation solution is vegetable oil.
[0008] Further, the heat treatment conditions in step S.2 are 235-245 h in an oven at 75-80°C.
[0009] Further, the specific data of the ICP-MS instrument in step S.4 are as follows: the count intensity of Be element is >4500, the count intensity of In element is >8000, and the count intensity of U element is >60000; the background technology intensity is ≤4; the oxide value is ≤2.5%; and the double charge value is ≤3.0%.
[0010] Further, the ICP-MS test in step S.4 has the following parameters: the plasma gas flow is 15-17 L / min, the auxiliary gas flow is 1.0-1.4 L / min, the atomizer flow is 1.00-1.04 L / min, and the frequency power is 1500-1700 W.
[0011] Further, in step S.5, 72 Ge is used for correction 52 Cr; 59 Co, 60 Ni; 45 Sc is used for correction 78 Se, 88 Sr, 90 Zr; 103 Rh is used for correction 121 Sb, 137 Ba; 185 Re is used for correction 205 Tl.
[0012] Further, in step S.5, the calculation formula is as follows, acid-containing cosmetic simulation solution: , X is the content of the element to be tested in the cosmetic simulation solution, mg / L; C is the mass concentration of the element to be tested in the cosmetic simulation solution, ug / L; C0 is the mass concentration of the element to be tested in the blank simulation solution, ug / L; and 1000 is the conversion coefficient; oil-containing cosmetic, alcohol-containing cosmetic simulation solution: , X is the content of the element to be detected in the cosmetic simulation liquid, mg / kg; C is the mass concentration of the element to be detected in the cosmetic simulation liquid, ug / L; C0 is the mass concentration of the element to be detected in the blank simulation liquid, ug / L; V is the constant volume of the cosmetic simulation liquid, mL; m is the mass of the cosmetic simulation liquid, g; and 1000 is a conversion coefficient.
[0013] The second aspect of the present application provides an application of a detection method of 9 kinds of metal migration amounts in cosmetic packaging materials in risk assessment of heavy metal migration in cosmetic packaging materials.
[0014] The present application has the following beneficial effects: (1) The present application can detect 9 kinds of elements at the same time, which can effectively improve the detection efficiency; the pretreatment method is designed according to different cosmetic simulation liquids, which is beneficial to improve the accuracy of detection.
[0015] (2) The present application has low detection limit and good precision, which is suitable for risk assessment of heavy metal migration in cosmetic packaging materials and meets the current safety supervision requirements.
[0016] (3) The present application is simple and time-saving, and is suitable for application in specific process flow. BRIEF DESCRIPTION OF DRAWINGS
[0017] Figure 1 is a process flow chart. DETAILED DESCRIPTION
[0018] The following will illustrate the embodiments of the present application through specific specific examples, and those skilled in the art can easily understand other advantages and effects of the present application from the disclosure of the present specification. The present application can also be implemented or applied by different specific embodiments, and the details in the specification can be modified or changed based on different views and applications without departing from the spirit of the present application. It should be noted that the following examples and features in the examples can be combined with each other without conflict. The methods used in the present application embodiments are conventional methods, and the reagents used can be obtained from commercial channels.
[0019] Example 1 A detection method of 9 kinds of metal migration amounts in cosmetic packaging materials: (S.1) Sample acquisition: Different types of cosmetic simulation liquids were taken. The cosmetics were divided into acid-containing cosmetic simulation liquids, alcohol-containing cosmetic simulation liquids, and oil-containing cosmetic simulation liquids. The acid-containing cosmetics included acid-containing cotton pads and acid-containing topical masks. The alcohol-containing cosmetics were divided into products with an alcohol content of <10% and products with an alcohol content of <80%. The products with an alcohol content of <10% included skin care products such as water and lotion, and the products with an alcohol content of <80% included various perfume products. The oil-containing cosmetics included lipsticks, facial oils, etc., as detailed in Table 1.
[0020] Table 1. Product Types Corresponding to Cosmetic Simulation Liquids
[0021] Given the complexity of cosmetic ingredients and their significant differences among different products, in order to accurately simulate the migration characteristics of cosmetics and packaging materials during actual contact, an analysis was conducted based on the specific solubility characteristics of cosmetic packaging materials and various factors affecting the leaching of heavy metals.
[0022] (S.2) Sample migration: Migration experiments were conducted on cosmetic packaging materials using a filling method. Simulated liquid was poured into the packaging material, with the liquid level 10 mm below the seal. The sealed plastic packaging material was then placed in an 80°C oven for 240 hours, and then removed for testing.
[0023] (S.3) Sample pretreatment: The acid-containing cosmetic simulation solution was filtered through a filter membrane.
[0024] Take 10g of alcohol-containing cosmetic simulation solution, heat it to near dryness, transfer it to a 10mL volumetric flask, and dilute to 10mL with 5% nitric acid. Filter the solution.
[0025] Weigh 0.5g of oil-containing cosmetic simulation solution into a polytetrafluoroethylene digestion vessel, add 6mL of nitric acid, heat for pre-digestion. After pre-digestion, remove the digestion vessel and cool to room temperature before microwave digestion. After digestion, heat until no yellow smoke is emitted, dilute to 25mL with deionized water, and filter.
[0026] (S.4) ICP-MS instrument was used for testing, data acquisition and processing: The instrument was tuned using an instrument tuning solution, and the analytical conditions were optimized to achieve the following: Be element count intensity > 4500, In element count intensity > 8000, U element count intensity > 60000; background technical intensity ≤ 4; oxide value ≤ 2.5%; double charge value ≤ 3.0%. The optimized instrument conditions are shown in Table 2 below.
[0027] Table 2 Instrument Operating Parameters
[0028] (S.5) Prepare standard solutions and calculate the content of each element: Based on the instrument conditions and element content levels, the concentrations of standard solutions for chromium, cobalt, nickel, selenium, strontium, antimony, barium, thallium, and zirconium are shown in Table 3.
[0029] Table 3 Concentration of Standard Solution Series
[0030] The selection criteria for internal standard elements are as follows: elements with mass numbers close to the analyte, comparable ionization energies, and extremely low or almost non-existent concentrations in the sample are selected as internal standards to correct for instrument signal drift and matrix effects. Specific pairings are as follows: 72 Ge is used for calibration. 52 Cr; 59 Co, 60 Ni; 45 Sc is used for correction 78 Se, 88 Sr, 90 Zr; 103 Rh is used for calibration. 121 Sb, 137 Ba; 185 Re is used for calibration. 205 Tl.
[0031] The calculation formula for the steps is as follows. Acid-containing cosmetic simulation solution: X represents the content of the element to be tested in the cosmetic simulation solution, mg / L; C represents the mass concentration of the element to be tested in the cosmetic simulation solution, ug / L; C0 represents the mass concentration of the element to be tested in the blank simulation solution, ug / L; 1000 is the conversion factor.
[0032] Oil-containing cosmetics, alcohol-containing cosmetic simulation liquids: X is the content of the element to be tested in the cosmetic simulation solution, mg / kg; C is the mass concentration of the element to be tested in the cosmetic simulation solution, ug / L; C0 is the mass concentration of the element to be tested in the blank simulation solution, ug / L; V is the final volume of the cosmetic simulation solution, mL; m is the mass of the cosmetic simulation solution weighed, g; 1000 is the conversion factor.
[0033] Example 2 Using commercially available metal packaging materials as experimental subjects, a migration experiment was conducted using a 4% acetic acid simulated solution. The materials were extracted at 80℃ for 10 days, and the simulated solution was then analyzed by ICP-MS. The measured migration amounts were 5.39 ug / L for chromium, 57.81 ug / L for nickel, and 36 ug / L for barium. The measurements were repeated six times, and the relative standard deviation was less than 4%.
[0034] Table 4 Relative Standard Deviation Test 。
Claims
1. A method for detecting the migration levels of nine metals in cosmetic packaging materials, characterized in that, The method includes the following steps: (S.1) Sample acquisition: Take cosmetic simulation solution, which is divided into acid-containing cosmetic simulation solution, alcohol-containing cosmetic simulation solution and oil-containing cosmetic simulation solution; (S.2) Sample migration: The cosmetic simulation liquid is filled into the packaging material of the cosmetic to be tested, sealed, and the sealed packaging material is heated. (S.3) Sample pretreatment: Take the cosmetic simulation solution in the packaging material and perform the following treatments respectively: filter the acid-containing cosmetic simulation solution through a filter membrane; heat the alcohol-containing cosmetic simulation solution to near dryness, make up to volume with nitric acid, and filter; add nitric acid to the oil-containing cosmetic simulation solution, heat and pre-digest, after pre-digestion, cool to room temperature, and then perform microwave digestion. After digestion, heat until no yellow smoke is emitted, make up to volume with deionized water, and filter. (S.4) ICP-MS instrument was used for testing, data acquisition and processing; (S.5) Prepare standard solutions and calculate the content of each element.
2. The method for detecting the migration levels of nine metals in cosmetic packaging materials as described in claim 1, characterized in that, The nine metals include chromium, cobalt, nickel, selenium, strontium, zirconium, antimony, barium, and thallium.
3. The method for detecting the migration levels of nine metals in cosmetic packaging materials as described in claim 1, characterized in that, The acid-containing cosmetic simulation solution is 4% acetic acid, the alcohol-containing cosmetic simulation solution is 10%-90% ethanol, and the oil-containing cosmetic simulation solution is vegetable oil.
4. The method for detecting the migration levels of nine metals in cosmetic packaging materials as described in claim 1, characterized in that, The heat treatment conditions in step S.2 are: 235-245 hours in an oven at 75℃-80℃.
5. The method for detecting the migration levels of nine metals in cosmetic packaging materials as described in claim 1, characterized in that, The specific data of the ICP-MS instrument in step S.4 are as follows: Be element count intensity > 4500, In element count intensity > 8000, U element count intensity > 60000; background technology intensity ≤ 4; oxide value ≤ 2.5%; double charge value ≤ 3.0%.
6. The method for detecting the migration levels of nine metals in cosmetic packaging materials as described in claim 1, characterized in that, In step S.4, during the ICP-MS test, the plasma gas flow rate is 15-17 L / min, the auxiliary gas flow rate is 1.0-1.4 L / min, the atomizer flow rate is 1.00-1.04 L / min, and the radio frequency power is 1500-1700 W.
7. The method for detecting the migration levels of nine metals in cosmetic packaging materials as described in claim 6, characterized in that, In step S.5, 72 Ge is used for calibration. 52 Cr; 59 Co, 60 Ni; 45 Sc is used for correction 78 Se, 88 Sr, 90 Zr; 103 Rh is used for calibration. 121 Sb, 137 Ba; 185 Re is used for correction. 205 Tl.
8. The method for detecting the migration levels of nine metals in cosmetic packaging materials as described in claim 1, characterized in that, The calculation formula in step S.5 is as follows: Acid-containing cosmetic simulation solution: X represents the content of the element to be tested in the cosmetic simulation solution, mg / L; C represents the mass concentration of the element to be tested in the cosmetic simulation solution, ug / L; C0 represents the mass concentration of the element to be tested in the blank simulation solution, ug / L; 1000 is the conversion factor. Oil-containing cosmetics, alcohol-containing cosmetic simulation liquids: X is the content of the element to be tested in the cosmetic simulation solution, mg / kg; C is the mass concentration of the element to be tested in the cosmetic simulation solution, ug / L; C0 is the mass concentration of the element to be tested in the blank simulation solution, ug / L; V is the final volume of the cosmetic simulation solution, mL; m is the mass of the cosmetic simulation solution weighed, g; 1000 is the conversion factor.
9. The application of the detection method for the migration of nine metals in cosmetic packaging materials as described in any one of claims 1-8 in the risk assessment of heavy metal migration in cosmetic packaging materials.