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Method for measuring ethanolamine substance residual quantity in cosmetics

A technology for ethanolamines and cosmetics, which is applied in the field of cosmetics detection, can solve the problems of high detection limit of monoethanolamine, high analysis precision, fast work efficiency, etc., and achieves the effects of high sensitivity, high extraction recovery rate and easy operation.

Inactive Publication Date: 2014-04-30
谱尼测试集团深圳有限公司
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  • Abstract
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  • Application Information

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Problems solved by technology

[0010] The technical problem to be solved in the present invention is mainly to solve the problem that the detection limit of monoethanolamine, diethanolamine and triethanolamine in cosmetics is higher and the sensitivity is lower in the existing method, and the high performance liquid chromatography-tandem mass spectrometry technology is used to accurately detect It is qualitative and quantitative, with high analysis precision and fast work efficiency

Method used

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  • Method for measuring ethanolamine substance residual quantity in cosmetics
  • Method for measuring ethanolamine substance residual quantity in cosmetics
  • Method for measuring ethanolamine substance residual quantity in cosmetics

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Using water as a solvent, prepare stock solutions of monoethanolamine, diethanolamine, and triethanolamine respectively according to Table 1, and prepare mixed standard solutions, and perform LC-MS / MS analysis and detection according to the above experimental conditions. figure 1 , figure 2 , image 3 The chromatograms in the figure are the extracted ion mass spectrograms of the three ethanolamines detected, respectively. The ordinate in the mass spectrogram represents the relative instrument corresponding value of the peak, and the abscissa is the retention time, and the unit is min. Make a graph with peak area to concentration, according to the measurement result of standard solution, set up the standard curve of three kinds of ethanolamines, such as Figure 4 As shown in the standard curve diagram, the abscissa in the standard curve diagram is the concentration of the target substance, and the ordinate is the response value of the liquid chromatography peak area. ...

Embodiment 2

[0048] Add the standard test solution among the example 1 with the emollient cream sample extraction solution of 0.2% (v / v) formic acid ethanol, wherein the concentration that contains standard solution is monoethanolamine, diethanolamine and triethanolamine is 1.0 μ g / mL, the test system For the precision, the measurement was repeated 6 times, and the analysis results are shown in Table 4. The relative standard deviation RSD of the repeated test was 2.2-3.4%, indicating that the stability of the instrument system was very good.

[0049] Table 4 Precision Test

[0050]

Embodiment 3

[0052] Blank test: Accurately weigh 2.00g of body cream samples into three 50mL plastic centrifuge tubes, add 20mL of 0.2% (v / v) formic acid ethanol solution into 50mL centrifuge tubes, first vortex and mix for 1min, then put into ultrasonic In the instrument, sonicate at room temperature for 5 minutes. Then refrigerate and centrifuge at 8000r / min at 4°C for 5min. After passing through a 0.22 μm filter membrane, it was tested by high-performance liquid chromatography-tandem mass spectrometry. Make three parallel samples of this sample, such as Figure 5 As shown, the target substance was not detected in the sample.

[0053] The recovery rate of standard addition of table 5 moisturizer cream sample

[0054]

[0055]

[0056] Spike recovery rate test: Accurately weigh 2.00g of moisturizer in parallel into three 50mL plastic centrifuge tubes, numbered Spike A, Spike B, and Spike C. Carry out the standard addition experiment of 3 concentration gradients to this sample, a...

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Abstract

The invention discloses a method for measuring ethanolamine substance residual quantity in cosmetics. The method comprises the following steps of detecting a sample which is subjected to liquid-liquid extraction by using high performance liquid chromatography-tandem mass spectrometry instrument (HPLC-MS / MS), adding a formic ethanol solution in the sample, uniformly mixing in a volution manner, carrying out ultrasound extraction and centrifugal separation, taking a supernatant fluid and detecting by using the HPLC-MS / MS. The liquid chromatography conditions are that an amino liquid chromatography pillar is adopted, the column temperature is 30-60 DEG C, sample volume is 10-20mu L and the flowing speed of a flowing phase is 0.15-0.60mL / min; and the MS / MS conditions include an electric atomizing ion source, an cation mode ionization and a multi-ion reaction monitoring mode (MRM). The method provided by the invention has the characteristics that the extraction and purification are rapid, the selectivity of the method is high, the specificity of a chromatogram is strong, the interference is small, and the detection limit is low.

Description

【Technical field】: [0001] The invention belongs to the technical field of cosmetic detection methods, and in particular relates to a method for determining residual amounts of monoethanolamine, diethanolamine and triethanolamine in cosmetics by using high performance liquid chromatography-tandem mass spectrometry. 【Background technique】: [0002] Ethanolamine is an important fine chemical raw material, mainly including monoethanolamine, diethanolamine, triethanolamine, etc. It is an important derivative of ethylene oxide and is widely used in polyurethane products, surfactants, medicine, gas purification, rubber It is an organic base commonly used in cosmetics in the fields of processing and textiles, and ethanolamine is also widely used as a pH balancer for various detergents and beauty and skin care products. The English names, CAS numbers, physical and chemical properties and uses of the three ethanolamines are introduced as follows: [0003] Monoethanolamine, English na...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 宋薇
Owner 谱尼测试集团深圳有限公司
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