Determination method of purity value and uncertainty of phenol and hydroquinone standard substance
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A technology for hydroquinone and standard substances is applied in the field of the development of standard substances for detecting the purity of phenolic compounds in freckle-removing cosmetics and shampoos, and can solve the problems of large differences and different test results, etc.
Active Publication Date: 2019-09-13
ZHEJIANG MEASUREMENT SCI RES INST
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At present, the quantitative detection of additives in cosmetics mostly adopts the direct detection method. However, in the actual application process, for the same sample, the test results provided by different testing agencies are not the same, or even have large differences.
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Embodiment 1
[0135] Example 1: Phenol
[0136] Step 1 - Raw Material Screening
[0137] The phenol raw material produced by Bailingwei Technology Co., Ltd. was used. Use the HPLC method (see step 3-1.2 of Example 1) to measure the purity value, and obtain the sample to be tested after the initial purity test is qualified after recrystallization twice.
[0138] Step 2 - Qualitative Confirmation
[0139] The phenol was confirmed qualitatively by GC-MS and FT-IR.
[0140] Step 2-1. Qualitative confirmation of phenol by GC-MS
[0141] For the phenol sample to be tested, it was dissolved in methanol to make a test solution, and the sample was injected for testing. The test conditions are as follows: set the inlet temperature to 250°C, the transfer line temperature to 280°C, the carrier gas flow rate to 1mL / min, the injection volume to 10μL, and the split ratio to 10:1; ℃, keep it for 1min, then raise the temperature to 270℃ at a rate of 15℃ / min, and keep it for 10min.
[0142] attached by...
Embodiment 2
[0207] Embodiment 2: hydroquinone
[0208] Step 1 Raw material screening
[0209] Through the commercially available hydroquinone raw material produced by Bailingwei Technology Co., Ltd. Use the HPLC method (see step 3-1.2 of Example 2) to measure the purity value, and obtain the sample to be tested after the initial purity test is qualified after recrystallization 3 times.
[0210] Step 2 - Qualitative Confirmation
[0211] Using GC-MS method and FT-IR method to qualitatively confirm hydroquinone.
[0212] Step 2-1, Qualitative confirmation of hydroquinone by GC-MS method
[0213] For the test sample of hydroquinone, dissolve it in methanol to make a test solution, and inject it for testing. The test conditions are as follows: set the inlet temperature to 250°C, the transfer line temperature to 280°C, the carrier gas flow rate to 1mL / min, the injection volume to 10μL, and the split ratio to 10:1; the temperature rise operation of the chromatographic column is: It is: use...
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Abstract
The invention discloses a method for measuring purity values and uncertainty degrees of standard substances of phenol and hydroquinone. The method comprises the following steps: screening raw materials for purity qualification; performing qualitative confirmation on to-be-measured samples by combining a gas chromatography-mass spectrometry with a Fourier transform infrared spectroscopy; measuring the purity of the to-be-measured samples by combining three methods different in principle including a GC method, an HPLC method and a DSC method; sub-packaging the to-be-measured samples; checking uniformity and stability; calculating to obtain the uncertainty degree caused by purity measurement; calculating the uncertainty degree caused by the uniformity and the stability according to step four; and synthesizing all the uncertainty degrees to obtain a total uncertainty degree. The method provided by the invention has accurate qualification, reduces system error, adopts a strict statistical data processing method and a comprehensive uncertainty degree evaluation method, ensures accuracy, stability and traceability of measured values, and obtains high-purity standard substances of phenol and hydroquinone.
Description
technical field [0001] The invention relates to the field of cosmetic testing, in particular to a method for developing a purity standard substance for detecting phenolic compounds in freckle-removing cosmetics and shampoos. The phenolic compounds mainly refer to phenol and hydroquinone. Background technique [0002] Accurate detection of additives in cosmetics is crucial to the safety of cosmetics. Since phenol and hydroquinone are banned substances in cosmetics, the difficulty of accurate detection of such trace additives is greatly increased. At present, the quantitative detection of additives in cosmetics mostly adopts the direct detection method. However, in the actual application process, for the same sample, the test results provided by different testing agencies are not the same, or even have large differences. Compared with standard compounds, additive standard substances in cosmetics not only have accurately measured or strictly defined standard values, but also ha...
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