Method for qualitative and quantitative analysis of titanium dioxide or/and zinc oxide nanoparticles in cosmetic

A zinc oxide nano, titanium dioxide technology, applied in particle size analysis, material analysis, particle and sedimentation analysis, etc., can solve the problems of cumbersome operation, time-consuming, poor recovery rate, etc., and achieve the effect of optimizing treatment conditions and the method is simple and fast

Inactive Publication Date: 2015-09-16
SUN YAT SEN UNIV +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above-mentioned methods all have problems such as poor recovery rate, or no verification of the loss of titanium dioxide content by the treatment method, and only a single qualitative or quantitative analysis is performed.
Patent CN201110235168.7 discloses a method for identifying and detecting nano-titanium dioxide in sunscreen cosmetics, which has the following defects: (1) Long processing time: the processing of n-hexane, chloroform, acetone, and methanol takes more than several hours for ultrasonic vibration and centrifugation, and Demulsification in the front water bath, the whole step is cumbersome and takes more than ten or even twenty hours
Using the sulfuric acid-nitric acid mixed acid system used in the inspection and quarantine industry standard to wet digest sunscreen also takes a long time, and samples with high mineral oil content even need to be digested for a day or two
(2) The solvent used is toxic and causes a large loss of the target analyte, titanium dioxide: the patent uses a variety of solvents

Method used

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  • Method for qualitative and quantitative analysis of titanium dioxide or/and zinc oxide nanoparticles in cosmetic
  • Method for qualitative and quantitative analysis of titanium dioxide or/and zinc oxide nanoparticles in cosmetic
  • Method for qualitative and quantitative analysis of titanium dioxide or/and zinc oxide nanoparticles in cosmetic

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0088] Example 1 Sample pretreatment solvent selection

[0089] 1. Extraction of nanoparticles in cosmetics

[0090] Different analytical instruments have certain requirements for the preparation of samples. Since cosmetics are mainly composed of organic matter and contain less inorganic nanoparticles, it is not possible to directly dry the cosmetics as they are and make them into powders for characterization and analysis of nanostructures. Combined with the sample preparation requirements of TEM, XRD, XPS and other characterization techniques, it is necessary to remove most of the organic matter in the cosmetics, and try not to lose the titanium dioxide or zinc oxide nanoparticles in the cosmetics.

[0091] The densities of nano titanium dioxide and zinc oxide are 3.8-4.3g / cm 3 and 5.6g / cm 3 , After adding an organic solvent and ultrasonically centrifuging, the organic matter is dissolved in the supernatant, and the nanoparticles are precipitated at the bottom, thereby re...

Embodiment 2

[0116] Qualitative and quantitative analysis of embodiment 2 titanium dioxide nanoparticles

[0117] 1. Qualitative and semi-quantitative analysis

[0118] 1. Sample preparation

[0119] S1. Sample number: 7 different brands of sunscreen and whitening products on the market are numbered 1-7, which are: sunscreen No. 1-3, liquid foundation No. 4-6, and pressed powder No. 7.

[0120] S2. Weigh about 0.3mg of the sample into a 10mL centrifuge tube, add 9mL of ethanol and let it stand for 2h to break the emulsification, ultrasonicate at 135w, 40kHZ for 5min, centrifuge at 10000r / min for 5min, and leave the precipitate;

[0121] S3. Add 9 mL of ethyl acetate to the precipitate obtained in S2, sonicate at 135w, 40kHZ for 5min, centrifuge at 10000r / min for 5min, remove most of the organic components and leave the precipitate; add 9mL of ethyl acetate again, and treat with 135w, 40kHZ for 5min , centrifuge at 10000r / min for 5min, and keep the precipitate;

[0122] S4. Finally, dr...

Embodiment 3

[0157] Qualitative and quantitative analysis of nano zinc oxide in the embodiment 3 cosmetics

[0158] 1. Qualitative and semi-quantitative analysis

[0159] 1. Sample preparation

[0160] Two commercially available sunscreen and whitening products of different brands are numbered: Sunscreen No. 8 and No. 9, and the pretreatment method is the same as in Example 1.

[0161] 2, TEM, XRD, XPS analysis method is the same as embodiment 1.

[0162] (1) Sample TEM characterization analysis results

[0163] The results are attached Figure 19 and 20 shown. The particles of No. 8 sunscreen have different shapes, including rod shape, round shape and other irregular shapes. The size range is between 6.5 nm and 88 nm, and the average size is 34.5 nm. The EDS spectrum shows that the main inorganic element is Zn.

[0164] Most of the particles of sunscreen No. 9 were round in shape, with a size range of 11.8 nm to 46.9 nm and an average size of 25.3 nm. EDS spectrum shows that the m...

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Abstract

The invention discloses a method for qualitative and quantitative analysis of titanium dioxide or/and zinc oxide nanoparticles in a cosmetic. The method includes: using ethyl acetate and ethanol to conduct dissolution and centrifugation treatment on the cosmetic to remove most organic components, performing drying, then conducting TEM, XRD and XPS analysis on the sample, observing the shape through TEM to obtain the particle size distribution so as to confirm whether a nano-material is added, performing XRD analysis to obtain the phase components and structure of the additive, and performing XPS to obtain the chemical form of elements; then combining ICP-OES quantitative determination to obtain the element content, thereby obtaining the content and morphological structure information of nano-components in the sample. The method can be used for detection of titanium dioxide or/and zinc oxide nanoparticles in cosmetics, and has the characteristics of small nanoparticle loss, accurate result, and safe operation process. Also the method provided by the invention has wide detection application range, is not only suitable for treatment of sun cream samples, and is also applicable to liquid foundations, compact powder and other sunscreen and whitening products.

Description

technical field [0001] The invention belongs to the technical field of nanoparticle substance detection, and more particularly relates to a method for qualitatively and quantitatively analyzing titanium dioxide or / and zinc oxide nanoparticles in cosmetics. Background technique [0002] Nanotechnology is a high-tech technology emerging at the end of the 20th century. It has been gradually applied in food, medicine, cosmetics and other fields in recent years. The International Organization for Standardization (ISO) proposed in ISO / TS 27687 that nanomaterials refer to materials with at least one dimension in the nanoscale range of 1 to 100 nm in three-dimensional space. The particle size of titanium dioxide nanomaterials is less than 100nm, which can effectively scatter and absorb ultraviolet rays, and has white color and good dispersibility. Therefore, it is widely added to sunscreen, foundation cream, lipstick, sunscreen mousse and other cosmetics. TiO in sunscreen cosmetics...

Claims

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Application Information

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IPC IPC(8): G01N15/00G01N15/02
Inventor 王素娟韦晓群龚力栾天罡刘洪涛相大鹏
Owner SUN YAT SEN UNIV
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