Method for simultaneously detecting 38 restricted coloring agents in cosmetic
A technology for colorants and cosmetics, applied in the field of detection, can solve the problems that the detection methods and means are difficult to meet the quality supervision requirements of restricted colorants, and achieve simple and easy extraction methods, simplified processing procedures, and simple and easy analysis operations. Effect
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preparation example Construction
[0079] (3) Preparation of sample solution
[0080] Take 0.2 g of the cosmetic sample to be tested in a centrifuge tube, add 6 mL of tetrahydrofuran, vortex and sonicate for 10 min to disperse the sample and extract the target substance, continue to add 2 mL of methanol and 2 mL of solution 2 to the centrifuge tube; then vortex Mix well by swirling, ultrasonically extract for 10 min, and then centrifuge at 5000 r / min for 10 min; take 2 mL of the upper layer extract in a 5 mL graduated plastic test tube, blow nitrogen to concentrate to about 0.5 mL, then dilute with methanol and dilute to 4 mL, after ultrasonication for 30 min, filtered through a PTFE membrane and transferred to an injection bottle for testing; if the lipstick sample cannot be dispersed, it can be dispersed by heating in an 80°C water bath for 1-2 min.
[0081] (4) Reference conditions for liquid chromatography analysis
[0082] Chromatographic column: ZORBAX SB-Aq, 3.5 μm, 3.0 mm×150 mm;
[0083] Column tempera...
example 1
[0107] Example 1, optimization of experimental method
[0108] (1) Optimization of sample pretreatment method
[0109] Considering the dispersibility of cosmetic samples and the solubility of the target substance, this experiment tried to use tetrahydrofuran as a dispersion solvent to disperse the sample and dissolve the target components, and then add polar methanol aqueous solution to increase the polarity of the system and make the non-polarity in the sample Components (such as the wax base in lipstick and the macromolecular excipient in nail polish) are separated out, so as to avoid the damage of these substances to the reversed-phase chromatographic column and prolong the service life of the chromatographic column. The addition of ammonium acetate can effectively improve the low yield of some target substances caused by matrix adsorption. By optimizing the dosage of tetrahydrofuran, methanol and ammonium acetate aqueous solution in the extraction system, the final optima...
example 2
[0120] Example 2, the inventive method verification experiment
[0121] (1) Linear range and correlation coefficient
[0122] A series of standard mixed solutions with concentrations of 10 μg / mL, 8 μg / mL, 6 μg / mL, 4 μg / mL, 2 μg / mL and 1 μg / mL were analyzed according to the optimized chromatographic conditions. The mass concentration is the abscissa, the peak area is the ordinate, and linear regression analysis is carried out. The linear regression equations and correlation coefficients of each target are shown in Table 3. The results showed that each target substance had a good linear relationship in the range of 1-10 μg / mL, and the correlation coefficients were all greater than 0.999.
[0123] Table 3 Standard curves and correlation coefficients of 38 restricted colorants
[0124]
[0125] (2) Recovery rate and lower limit of quantitation
[0126]Quantitatively add standard stock solutions A, B, C, D and E to the blank sample without the target substance, perform detec...
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