CN113358793A - Method for detecting content of preservative in cosmetics - Google Patents
Method for detecting content of preservative in cosmetics Download PDFInfo
- Publication number
- CN113358793A CN113358793A CN202110704664.6A CN202110704664A CN113358793A CN 113358793 A CN113358793 A CN 113358793A CN 202110704664 A CN202110704664 A CN 202110704664A CN 113358793 A CN113358793 A CN 113358793A
- Authority
- CN
- China
- Prior art keywords
- preservative
- solution
- detecting
- cosmetic
- standard
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/08—Preparation using an enricher
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Cosmetics (AREA)
Abstract
The invention belongs to the technical field of preservative determination, and discloses a method for detecting the content of a preservative in cosmetics, which comprises the following steps: pretreating the cosmetics to be detected to obtain a cosmetic extracting solution to be detected, and purifying and enriching the obtained cosmetic extracting solution by using an ultrafiltration membrane; preparing standard solutions of various preservatives, mixing the standard solutions of various preservatives, and diluting the standard solutions with methanol solutions according to different multiples to prepare 8 standard solutions to obtain mixed standard solutions; and detecting by using a high performance liquid image chromatography to obtain a standard curve of the mixed standard solution, detecting the cosmetic solution after purification and enrichment treatment by using the high performance liquid image chromatography, and comparing with the standard curve to obtain a preservative detection result. The method can be used for simply, conveniently and efficiently extracting the preservative in the cosmetics and enriching the preservative, so that the detection sensitivity is improved, and the accuracy and efficiency of detection are ensured. The invention can detect various preservatives, and has low detection cost and high detection efficiency.
Description
Technical Field
The invention belongs to the technical field of preservative determination, and particularly relates to a method for detecting the content of a preservative in cosmetics.
Background
At present, various nutrient substances are added into cosmetics, and the nutrient substances are culture mediums for microbial propagation, so that the products can generate peculiar smell or change the appearance due to bacterial pollution in the production, use and storage of the cosmetics, and a certain amount of preservative is added into the products for inhibiting the growth and propagation of bacteria, but the constant contact can cause adverse effects on the health of human bodies. The content measurement of the preservative in the cosmetics is a method for evaluating the safety, rapidness, simplicity and directness of the use of the preservative in the cosmetics. At present, the detection of preservatives in cosmetics mainly adopts liquid chromatography and gas chromatography tandem mass spectrometry as mainstream, but the existing detection method has low detection efficiency and high cost and cannot detect a plurality of preservatives simultaneously. Therefore, a new method for detecting the content of the preservative in the cosmetic is needed.
Through the above analysis, the problems and defects of the prior art are as follows: the existing detection method has low detection efficiency and high cost, and can not detect various preservatives simultaneously.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method for detecting the content of a preservative in cosmetics.
The invention is realized by a method for detecting the content of a preservative in cosmetics, which comprises the following steps:
step one, preparing a mesoporous magnetic graphene composite material with a modification function: synthesizing 3-glycidoxypropyltrimethoxysilane GLYMO-aminophenylboronic acid APB: carrying out reaction feeding at low temperature, then heating for reaction, and connecting GLYMO with APB; uniformly dispersing graphene in concentrated nitric acid for acidification treatment, performing reactive modification on the surface of the obtained acidified graphene to obtain magnetic graphene by using ferroferric oxide microspheres, and coating mesoporous silicon on the magnetic graphene by one step; adding a mesoporous magnetic graphene composite material into a GLYMO-APB solution, and heating to react to finish modification of the material to prepare the mesoporous magnetic graphene composite material with the modification function for later use;
step two, pretreating the cosmetics to be detected to obtain the cosmetic extracting solution to be detected: taking a proper amount of cosmetics to be detected containing a preservative; adding the cosmetic to be tested into an ammonium acetate aqueous solution, keeping the temperature constant at 15-25 ℃, and slowly and uniformly stirring under the condition of least water evaporation to obtain a mixed solution; adding methanol into the obtained mixed solution after vortex, adjusting the pH value by using a pH regulator, absorbing supernatant after homogenizing, ultrasonic and high-speed centrifugation, and extracting the supernatant by using ionic liquid to obtain a to-be-detected cosmetic extracting solution containing a preservative for later use;
and step three, purifying and enriching the obtained cosmetic extracting solution by using an ultrafiltration membrane: purifying the cosmetic extracting solution containing the preservative to be detected by a 0.45-micrometer filter membrane to obtain a purified solution; adding a pre-synthesized modified mesoporous magnetic graphene composite material into the obtained purified liquid, and carrying out ultrasonic or vortex mixing for 15-20 min; separating out the material under the action of a magnetic field, removing the supernatant, adding an eluent into the material, and ultrasonically eluting for 15-20min to obtain a purified solution subjected to preservative enrichment for later use;
step four, detecting the purified and enriched cosmetic solution by using a high performance liquid image chromatography: opening and operating the high performance liquid chromatography system to set parameters; preparing an online cleaning and degassing device and starting the online cleaning and degassing device; cleaning a mobile phase-liquid phase system, installing a proper chromatographic column on a chromatographic instrument, and flushing the chromatographic column at the flow rate of 1mL/min for 30-35 min; adding cetyltrimethylammonium chloride into the mobile phase until the final concentration is 0.002moL, adjusting the pH value to 3.5 by using phosphoric acid, changing into a liquid phase system, washing a chromatographic column at the flow rate of 1mL/min, and sampling and testing after the base line of a chromatogram is stable for 10-20min to obtain a detection curve for detecting the purified and enriched cosmetic solution by using a high performance liquid chromatography;
preparing standard solutions of various preservatives, mixing the standard solutions of various preservatives to enable the concentration of each substance to be 100mg/L, and diluting the standard solutions with methanol solutions according to different multiples of 1, 2, 4, 6, 8, 10, 20 and 40 to prepare 8 standard solutions to obtain mixed standard solutions;
and step six, detecting by using a high-efficiency liquid-image chromatography to obtain a standard curve of the mixed standard solution, and comparing the detection curve of the cosmetic solution subjected to the purification and enrichment treatment by using the high-efficiency liquid-image chromatography with the standard curve to obtain a preservative detection result.
Further, in the first step, the reaction feeding at a low temperature and then the temperature rise reaction comprise:
dripping 10-150 mu L of GLYMO into the APB solution at low temperature, raising the temperature of the reaction system to 20-80 ℃, and stirring for reacting for 3-10 h.
Further, in the second step, the preservative is one or more of phenol, benzyl alcohol, methyl benzoate, ethyl benzoate, methyl paraben, ethyl paraben, propyl paraben, butyl paraben and isobutyl paraben.
Further, in the second step, the concentration of the ammonium acetate aqueous solution is 70mmol/L, and the dosage is 5 mL.
Further, in step two, the high-speed centrifugation comprises: 6000-14000 r/min, and 5-10min of centrifugation.
Further, in the second step, the extracting the supernatant with an ionic liquid includes:
taking the supernatant, adding 1-butyl-3-methylimidazole tetrafluoroborate, uniformly stirring, and then adding ammonium hexafluorophosphate aqueous solution.
Further, in step four, the setting of the parameters includes: setting the flow rate of a chromatographic pump to be 1 mL/min; the detection wavelength of the detector is 254 nm; the sampling frequency is 10 Hz; the column oven temperature was set at 40 ℃.
Further, in the fourth step, the chromatographic column is an ACQUITY UPLC BEH C8 chromatographic column;
the mobile phase is a mixture of A, B; wherein A is acetonitrile; the B is 5mmol/L ammonium acetate solution;
the mass spectrum conditions are as follows: the ion source is an electrospray ion source; the scanning mode is positive ion scanning.
Further, in step five, the preparing of the standard solution of the plurality of preservatives includes:
preparing a preservative standard product stock solution A: respectively and precisely weighing 0.2500g of 2-bromo-2-nitropropane-1, 3-diol, 0.2500g of benzyl alcohol, 0.1000g of phenoxyethanol, 0.1000g of benzoic acid, 0.0250g of isobutyl 4-hydroxybenzoate and 0.0250g of butyl 4-hydroxybenzoate into 10mL volumetric flasks, adding methanol to the scales, and uniformly mixing;
preparing a preservative standard substance stock solution B: respectively and precisely weighing 0.0500g of 4-hydroxybenzoic acid methyl ester, 0.0500g of 4-hydroxybenzoic acid ethyl ester, 0.0500g of 4-hydroxybenzoic acid isopropyl ester and 0.0500g of 4-hydroxybenzoic acid propyl ester into a 50mL volumetric flask, adding methanol to the scale, and uniformly mixing.
Further, in step five, the mixing of the standard solutions of the preservatives comprises:
mixing standard solutions of chlorphenesin and lorammonium chloride, and then diluting to obtain a first mixed standard solution;
and mixing the methyl paraben, propyl paraben and isopropyl paraben standard solutions, and then diluting to obtain a second mixed standard solution.
By combining all the technical schemes, the invention has the advantages and positive effects that: the method for detecting the content of the preservative in the cosmetics, provided by the invention, can be used for simply, conveniently and efficiently extracting the preservative in the cosmetics effectively, enriching the preservative, improving the detection sensitivity and ensuring the accuracy and efficiency of detection. The invention can detect various preservatives, and has low detection cost and high detection efficiency.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings needed to be used in the embodiments of the present application will be briefly described below, and it is obvious that the drawings described below are only some embodiments of the present application, and it is obvious for those skilled in the art that other drawings can be obtained from the drawings without creative efforts.
FIG. 1 is a flow chart of a method for detecting the content of a preservative in a cosmetic provided by an embodiment of the invention.
Fig. 2 is a flowchart of a method for preparing a mesoporous magnetic graphene composite material with a modification function according to an embodiment of the present invention.
Fig. 3 is a flowchart of a method for obtaining a cosmetic extracting solution to be tested after pre-treating a cosmetic to be tested according to an embodiment of the present invention.
Fig. 4 is a flowchart of a method for purifying and enriching the obtained cosmetic extracting solution by using an ultrafiltration membrane according to an embodiment of the present invention.
FIG. 5 is a flow chart of a method for detecting a cosmetic solution after purification and enrichment treatment by high performance liquid chromatography according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In view of the problems in the prior art, the present invention provides a method for detecting the content of preservative in cosmetics, and the present invention is described in detail below with reference to the accompanying drawings.
As shown in fig. 1, the method for detecting the content of the preservative in the cosmetic provided by the embodiment of the invention comprises the following steps:
s101, preparing a mesoporous magnetic graphene composite material with a modification function;
s102, pretreating the cosmetics to be detected to obtain the extracting solution of the cosmetics to be detected;
s103, purifying and enriching the obtained cosmetic extracting solution by using an ultrafiltration membrane;
s104, detecting the purified and enriched cosmetic solution by using a high performance liquid chromatography;
s105, preparing standard solutions of various preservatives, mixing the standard solutions of various preservatives to enable the concentration of each substance to be 100mg/L, and diluting the standard solutions with methanol solutions according to different multiples of 1, 2, 4, 6, 8, 10, 20 and 40 to prepare 8 standard solutions to obtain mixed standard solutions;
s106, detecting by using the high-efficiency liquid-image chromatography to obtain a standard curve of the mixed standard solution, and comparing the detection curve of the cosmetic solution subjected to the purification and enrichment treatment by using the high-efficiency liquid-image chromatography with the standard curve to obtain a preservative detection result.
As shown in fig. 2, in step S101 provided in the embodiment of the present invention, the preparing the mesoporous magnetic graphene composite material with the modification function includes:
s201, synthesizing 3-glycidoxypropyltrimethoxysilane GLYMO-aminobenzeneboronic acid APB: carrying out reaction feeding at low temperature, then heating for reaction, and connecting GLYMO with APB;
s202, uniformly dispersing graphene in concentrated nitric acid for acidification treatment, performing reactive modification on the surface of the obtained acidified graphene to obtain magnetic graphene by ferroferric oxide microspheres, and coating mesoporous silicon;
s203, adding the mesoporous magnetic graphene composite material into the GLYMO-APB solution, and heating to react to finish modification of the material to prepare the mesoporous magnetic graphene composite material with the modification function.
The method for carrying out reaction feeding at low temperature and then heating reaction provided by the embodiment of the invention comprises the following steps: dripping 10-150 mu L of GLYMO into the APB solution at low temperature, raising the temperature of the reaction system to 20-80 ℃, and stirring for reacting for 3-10 h.
As shown in fig. 3, in step S102 provided in the embodiment of the present invention, the pre-processing the cosmetic to be tested to obtain the cosmetic extracting solution to be tested includes:
s301, taking a proper amount of cosmetics to be detected containing preservatives;
s302, adding the cosmetic to be tested into an ammonium acetate aqueous solution, keeping the temperature constant at 15-25 ℃, and slowly and uniformly stirring under the condition of least water evaporation to obtain a mixed solution;
s303, adding methanol into the obtained mixed solution after vortex, adjusting the pH value by using a pH regulator, absorbing supernate after homogenization, ultrasound and high-speed centrifugation, and extracting the supernate by using ionic liquid to obtain the to-be-detected cosmetic extracting solution containing the preservative.
The preservative provided by the embodiment of the invention is one or more of phenol, benzyl alcohol, methyl benzoate, ethyl benzoate, methyl paraben, ethyl paraben, propyl paraben, butyl paraben and isobutyl paraben.
The concentration of the ammonium acetate aqueous solution provided by the embodiment of the invention is 70mmol/L, and the dosage is 5 mL.
The high-speed centrifugation provided by the embodiment of the invention comprises: 6000-14000 r/min, and 5-10min of centrifugation.
The method for extracting the supernatant by using the ionic liquid provided by the embodiment of the invention comprises the following steps: taking the supernatant, adding 1-butyl-3-methylimidazole tetrafluoroborate, uniformly stirring, and then adding ammonium hexafluorophosphate aqueous solution.
As shown in fig. 4, in step S103 provided in the embodiment of the present invention, the performing purification and enrichment treatment on the obtained cosmetic extracting solution by using an ultrafiltration membrane includes:
s401, purifying the cosmetic extracting solution containing the preservative to be detected by a 0.45-micrometer filter membrane to obtain a purified solution;
s402, adding a pre-synthesized modified mesoporous magnetic graphene composite material into the obtained purified liquid, and carrying out ultrasonic or vortex mixing for 15-20 min;
and S403, separating out the material under the action of a magnetic field, discarding the supernatant, adding eluent into the material, and performing ultrasonic elution for 15-20min to obtain the purified liquid subjected to preservative enrichment.
As shown in fig. 5, in step S104, the detecting, by using high performance liquid chromatography, the cosmetic solution after the purification and enrichment treatment includes:
s501, opening and operating a high performance liquid chromatography system to set parameters; preparing an online cleaning and degassing device and starting the online cleaning and degassing device;
s502, cleaning a mobile phase liquid phase system, installing a proper chromatographic column on a chromatographic instrument, and flushing the chromatographic column at the flow rate of 1mL/min for 30-35 min;
s503, adding cetyltrimethylammonium chloride into the mobile phase until the final concentration is 0.002moL, adjusting the pH value to 3.5 by using phosphoric acid, changing the mobile phase into a liquid phase system, washing the chromatographic column at the flow rate of 1mL/min, injecting and testing after the base line of the chromatogram is stable for 10-20min, and thus obtaining the detection curve of the cosmetic solution after the purification and enrichment treatment by using the high performance liquid chromatography.
In step S104 provided in the embodiment of the present invention, the parameter setting includes: setting the flow rate of a chromatographic pump to be 1 mL/min; the detection wavelength of the detector is 254 nm; the sampling frequency is 10 Hz; the column oven temperature was set at 40 ℃.
In step S104 provided by the embodiment of the present invention, the chromatographic column is an acquired uplc BEH C8 chromatographic column; the mobile phase is a mixture of A, B; wherein A is acetonitrile; the B is 5mmol/L ammonium acetate solution; the mass spectrum conditions are as follows: the ion source is an electrospray ion source; the scanning mode is positive ion scanning.
In step S105 provided in the embodiment of the present invention, the preparing a standard solution of multiple preservatives includes:
(1) preparing a preservative standard product stock solution A: respectively and precisely weighing 0.2500g of 2-bromo-2-nitropropane-1, 3-diol, 0.2500g of benzyl alcohol, 0.1000g of phenoxyethanol, 0.1000g of benzoic acid, 0.0250g of isobutyl 4-hydroxybenzoate and 0.0250g of butyl 4-hydroxybenzoate into 10mL volumetric flasks, adding methanol to the scales, and uniformly mixing;
(2) preparing a preservative standard substance stock solution B: respectively and precisely weighing 0.0500g of 4-hydroxybenzoic acid methyl ester, 0.0500g of 4-hydroxybenzoic acid ethyl ester, 0.0500g of 4-hydroxybenzoic acid isopropyl ester and 0.0500g of 4-hydroxybenzoic acid propyl ester into a 50mL volumetric flask, adding methanol to the scale, and uniformly mixing.
In step S105 provided in the embodiment of the present invention, mixing multiple standard solutions of preservatives includes: mixing standard solutions of chlorphenesin and lorammonium chloride, and then diluting to obtain a first mixed standard solution; and mixing the methyl paraben, propyl paraben and isopropyl paraben standard solutions, and then diluting to obtain a second mixed standard solution.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention, and the scope of the present invention is not limited thereto, and any modification, equivalent replacement, and improvement made by those skilled in the art within the technical scope of the present invention disclosed herein, which is within the spirit and principle of the present invention, should be covered by the present invention.
Claims (10)
1. A method for detecting the content of a preservative in a cosmetic is characterized by comprising the following steps of:
step one, preparing a mesoporous magnetic graphene composite material with a modification function: synthesizing 3-glycidoxypropyltrimethoxysilane GLYMO-aminophenylboronic acid APB: carrying out reaction feeding at low temperature, then heating for reaction, and connecting GLYMO with APB; uniformly dispersing graphene in concentrated nitric acid for acidification treatment, performing reactive modification on the surface of the obtained acidified graphene to obtain magnetic graphene by using ferroferric oxide microspheres, and coating mesoporous silicon on the magnetic graphene by one step; adding a mesoporous magnetic graphene composite material into a GLYMO-APB solution, and heating to react to finish modification of the material to prepare the mesoporous magnetic graphene composite material with the modification function for later use;
step two, pretreating the cosmetics to be detected to obtain the cosmetic extracting solution to be detected: taking a proper amount of cosmetics to be detected containing a preservative; adding the cosmetic to be tested into an ammonium acetate aqueous solution, keeping the temperature constant at 15-25 ℃, and slowly and uniformly stirring under the condition of least water evaporation to obtain a mixed solution; adding methanol into the obtained mixed solution after vortex, adjusting the pH value by using a pH regulator, absorbing supernatant after homogenizing, ultrasonic and high-speed centrifugation, and extracting the supernatant by using ionic liquid to obtain a to-be-detected cosmetic extracting solution containing a preservative for later use;
and step three, purifying and enriching the obtained cosmetic extracting solution by using an ultrafiltration membrane: purifying the cosmetic extracting solution containing the preservative to be detected by a 0.45-micrometer filter membrane to obtain a purified solution; adding a pre-synthesized modified mesoporous magnetic graphene composite material into the obtained purified liquid, and carrying out ultrasonic or vortex mixing for 15-20 min; separating out the material under the action of a magnetic field, removing the supernatant, adding an eluent into the material, and ultrasonically eluting for 15-20min to obtain a purified solution subjected to preservative enrichment for later use;
step four, detecting the purified and enriched cosmetic solution by using a high performance liquid image chromatography: opening and operating the high performance liquid chromatography system to set parameters; preparing an online cleaning and degassing device and starting the online cleaning and degassing device; cleaning a mobile phase-liquid phase system, installing a proper chromatographic column on a chromatographic instrument, and flushing the chromatographic column at the flow rate of 1mL/min for 30-35 min; adding cetyltrimethylammonium chloride into the mobile phase until the final concentration is 0.002moL, adjusting the pH value to 3.5 by using phosphoric acid, changing into a liquid phase system, washing a chromatographic column at the flow rate of 1mL/min, and sampling and testing after the base line of a chromatogram is stable for 10-20min to obtain a detection curve for detecting the purified and enriched cosmetic solution by using a high performance liquid chromatography;
preparing standard solutions of various preservatives, mixing the standard solutions of various preservatives to enable the concentration of each substance to be 100mg/L, and diluting the standard solutions with methanol solutions according to different multiples of 1, 2, 4, 6, 8, 10, 20 and 40 to prepare 8 standard solutions to obtain mixed standard solutions;
and step six, detecting by using a high-efficiency liquid-image chromatography to obtain a standard curve of the mixed standard solution, and comparing the detection curve of the cosmetic solution subjected to the purification and enrichment treatment by using the high-efficiency liquid-image chromatography with the standard curve to obtain a preservative detection result.
2. The method for detecting the content of the preservative in the cosmetic according to claim 1, wherein in the first step, the reaction feeding is performed at a low temperature and then the temperature rise reaction is performed, and the method comprises the following steps:
dripping 10-150 mu L of GLYMO into the APB solution at low temperature, raising the temperature of the reaction system to 20-80 ℃, and stirring for reacting for 3-10 h.
3. The method for detecting the content of the preservative in the cosmetic according to claim 1, wherein in the second step, the preservative is one or more of phenol, benzyl alcohol, methyl benzoate, ethyl benzoate, methyl paraben, ethyl paraben, propyl paraben, butyl paraben and isobutyl paraben.
4. The method for detecting the content of preservatives in cosmetics according to claim 1, wherein in the second step, the concentration of the aqueous solution of ammonium acetate is 70mmol/L and the amount is 5 mL.
5. The method for detecting the content of a preservative in a cosmetic according to claim 1, wherein in the second step, the high-speed centrifugation comprises: 6000-14000 r/min, and 5-10min of centrifugation.
6. The method for detecting the content of the preservative in the cosmetic according to claim 1, wherein in the second step, the supernatant is extracted by using an ionic liquid, and the method comprises the following steps:
taking the supernatant, adding 1-butyl-3-methylimidazole tetrafluoroborate, uniformly stirring, and then adding ammonium hexafluorophosphate aqueous solution.
7. The method for detecting the content of preservatives in cosmetics according to claim 1, wherein in step four, the parameter setting includes: setting the flow rate of a chromatographic pump to be 1 mL/min; the detection wavelength of the detector is 254 nm; the sampling frequency is 10 Hz; the column oven temperature was set at 40 ℃.
8. The method for detecting the content of preservatives in cosmetics according to claim 1, wherein in step four, the chromatographic column is an acquisition UPLC BEH C8 chromatographic column;
the mobile phase is a mixture of A, B; wherein A is acetonitrile; the B is 5mmol/L ammonium acetate solution;
the mass spectrum conditions are as follows: the ion source is an electrospray ion source; the scanning mode is positive ion scanning.
9. The method for detecting the content of the preservative in the cosmetic according to claim 1, wherein in the fifth step, the preparing of the standard solution of the plurality of preservatives comprises:
preparing a preservative standard product stock solution A: respectively and precisely weighing 0.2500g of 2-bromo-2-nitropropane-1, 3-diol, 0.2500g of benzyl alcohol, 0.1000g of phenoxyethanol, 0.1000g of benzoic acid, 0.0250g of isobutyl 4-hydroxybenzoate and 0.0250g of butyl 4-hydroxybenzoate into 10mL volumetric flasks, adding methanol to the scales, and uniformly mixing;
preparing a preservative standard substance stock solution B: respectively and precisely weighing 0.0500g of 4-hydroxybenzoic acid methyl ester, 0.0500g of 4-hydroxybenzoic acid ethyl ester, 0.0500g of 4-hydroxybenzoic acid isopropyl ester and 0.0500g of 4-hydroxybenzoic acid propyl ester into a 50mL volumetric flask, adding methanol to the scale, and uniformly mixing.
10. The method for detecting the content of preservatives in cosmetics according to claim 1, wherein in step five, the plurality of preservative standard solutions are mixed, and the method comprises the following steps:
mixing standard solutions of chlorphenesin and lorammonium chloride, and then diluting to obtain a first mixed standard solution;
and mixing the methyl paraben, propyl paraben and isopropyl paraben standard solutions, and then diluting to obtain a second mixed standard solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110704664.6A CN113358793A (en) | 2021-06-24 | 2021-06-24 | Method for detecting content of preservative in cosmetics |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110704664.6A CN113358793A (en) | 2021-06-24 | 2021-06-24 | Method for detecting content of preservative in cosmetics |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113358793A true CN113358793A (en) | 2021-09-07 |
Family
ID=77536163
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110704664.6A Pending CN113358793A (en) | 2021-06-24 | 2021-06-24 | Method for detecting content of preservative in cosmetics |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113358793A (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013014538A2 (en) * | 2011-07-25 | 2013-01-31 | American University In Cairo | Single-domain antibodies and graphene coated magnetic metal nanoparticles conjugate and methods for using the same |
| CN107478731A (en) * | 2016-06-07 | 2017-12-15 | 复旦大学 | The pre-treating method of parabens preservative in a kind of detection cosmetics |
| CN107664667A (en) * | 2017-09-23 | 2018-02-06 | 广州智妥科技有限公司 | A kind of assay method of Determination of Preservatives in Cosmetics content |
| WO2019233582A1 (en) * | 2018-06-07 | 2019-12-12 | Robert Bosch Gmbh | Porous materials based solid phase extraction of analyte from beverages |
| CN111060613A (en) * | 2019-12-13 | 2020-04-24 | 上海微谱化工技术服务有限公司 | Method for analyzing and detecting preservative in cosmetics |
| CN111474248A (en) * | 2019-12-19 | 2020-07-31 | 沈阳药科大学 | Method for determining four preservatives in cosmetics |
| US20200284856A1 (en) * | 2017-10-06 | 2020-09-10 | Jin Zhang | Giant magnetoresistance-based biosensors |
| CN112147210A (en) * | 2020-09-25 | 2020-12-29 | 复旦大学 | Preparation method, product and application of boric acid functionalized mesoporous graphene-silicon dioxide composite material |
-
2021
- 2021-06-24 CN CN202110704664.6A patent/CN113358793A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013014538A2 (en) * | 2011-07-25 | 2013-01-31 | American University In Cairo | Single-domain antibodies and graphene coated magnetic metal nanoparticles conjugate and methods for using the same |
| CN107478731A (en) * | 2016-06-07 | 2017-12-15 | 复旦大学 | The pre-treating method of parabens preservative in a kind of detection cosmetics |
| CN107664667A (en) * | 2017-09-23 | 2018-02-06 | 广州智妥科技有限公司 | A kind of assay method of Determination of Preservatives in Cosmetics content |
| US20200284856A1 (en) * | 2017-10-06 | 2020-09-10 | Jin Zhang | Giant magnetoresistance-based biosensors |
| WO2019233582A1 (en) * | 2018-06-07 | 2019-12-12 | Robert Bosch Gmbh | Porous materials based solid phase extraction of analyte from beverages |
| CN111060613A (en) * | 2019-12-13 | 2020-04-24 | 上海微谱化工技术服务有限公司 | Method for analyzing and detecting preservative in cosmetics |
| CN111474248A (en) * | 2019-12-19 | 2020-07-31 | 沈阳药科大学 | Method for determining four preservatives in cosmetics |
| CN112147210A (en) * | 2020-09-25 | 2020-12-29 | 复旦大学 | Preparation method, product and application of boric acid functionalized mesoporous graphene-silicon dioxide composite material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Han et al. | Analysis of some β-Lactam antibiotics using ionic liquids as mobile phase additives by RP-HPLC | |
| CN105181866A (en) | Method for rapid detection of benzalkonium chloride in eye drops | |
| CN108051517A (en) | The automated detection method of cumarin in a kind of electronic cigarette liquid | |
| Sochorova et al. | Electrochemical and others techniques for the determination of malic acid and tartaric acid in must and wine | |
| CN113358793A (en) | Method for detecting content of preservative in cosmetics | |
| CN113533548B (en) | Method for detecting 1-vinyl imidazole in chemical product | |
| CN111413432B (en) | Method for detecting trace PFOA (perfluorooctanoic acid) in fluorine-containing polymer emulsion product | |
| CN111077195B (en) | System and method for automatically measuring exchange capacity of strongly basic anion exchange resin | |
| CN102507757A (en) | Method for measuring ascorbic acid content in porphyra yezoensis by high performance liquid chromatography | |
| CN111220733A (en) | Method for determining L-carnosine by efficient capillary electrophoresis and application of method to quality evaluation of polaprezinc | |
| CN114609295A (en) | High performance liquid chromatography analysis method for quinic acid content in tala enzymolysis waste liquid | |
| CN102338779A (en) | Method for detecting sorbic acid content in cheese | |
| CN112505190B (en) | Method for detecting acrylic acid in soil | |
| CN109254104A (en) | The detection method of residues of organophosphate pesticides in a kind of grape wine | |
| CN112505223B (en) | Method for simultaneously detecting content of toxoflavin and content of mirostrobin in food | |
| Zhong et al. | Multi-channel purge and trap system coupled with ion chromatography for the determination of alkylamines in cosmetics | |
| CN108918694B (en) | HPLC pre-column derivatization detection method for MSX residues | |
| CN106290591A (en) | A kind of detection method of Gentamicin C1a | |
| CN112924566B (en) | Method for simultaneously detecting glycine and serine in enzymatic reaction liquid | |
| CN106383181A (en) | Method for detection of valine content in fermentation broth by precolumn derivatization-high performance liquid chromatography | |
| Acevedo et al. | A new SPME thermal desorption interface for HPLC | |
| CN104833760A (en) | Method for using high-performance liquid chromatography to measure greenhouse tomato soil low-molecular-weight organic acids | |
| CN111157666A (en) | Method for simultaneously and quantitatively analyzing sulfite and sulfate ions in amine solution | |
| CN110389187A (en) | The detection method of 4-HBA substance in a kind of cosmetics | |
| CN112198236B (en) | Method for detecting content of citrulline in citrulline raw material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |