CN215005145U - Detection apparatus for crotonic acid content in survey cosmetics - Google Patents
Detection apparatus for crotonic acid content in survey cosmetics Download PDFInfo
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- CN215005145U CN215005145U CN202021821583.1U CN202021821583U CN215005145U CN 215005145 U CN215005145 U CN 215005145U CN 202021821583 U CN202021821583 U CN 202021821583U CN 215005145 U CN215005145 U CN 215005145U
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Abstract
The utility model provides a detection apparatus for crotonic acid content in survey cosmetics, include: the device comprises a sampling mechanism, a preprocessing mechanism, a measuring mechanism and a data processing mechanism; the sampling mechanism comprises a sampling scale; the pretreatment mechanism comprises a colorimetric tube with a plug, a vortex oscillator, an ultrasonic extractor and a filter; a colorimetric tube with a plug and arranged in the vortex oscillator is provided with ethanol and a sample to prepare a mixed solution; placing the mixed solution in an extraction container of an ultrasonic extractor; filtering the mixed solution by a filter, and filling the mixed solution into a chromatographic column in a measuring mechanism; the output end of the measuring mechanism is electrically connected to the data processing mechanism. The utility model has the advantages of low detection limit, 1mg/kg of specific detection limit, easy acquisition of equipment, simple use, accurate detection and high popularization; by performing a standard addition recovery test on a typical cosmetic sample, the recovery rate is in the range of 80-110%; has good repeatability and reproducibility.
Description
Technical Field
The utility model relates to a crotonic acid content testing technical field especially relates to a detection device of crotonic acid content in survey cosmetics.
Background
Crotonic acid is an important chemical raw material, crotonic acid and derivatives thereof are often used as comonomers in the production process of rubber, latex, adsorbents and plastics, and water-soluble resins obtained by neutralizing crotonic acid-vinyl acetate copolymers can be further used as cosmetic raw materials in the formulations of shampoos, gel water, hair sprays and the like. However, crotonic acid has strong irritation to intestines and stomach and has paralysis effect on respiratory center and heart.
Although the related national industry standards do not have the limit requirements of the crotonic acid at all times, the crotonaldehyde is a forbidden component specified in the technical Specification for cosmetic safety, and the crotonaldehyde is gradually oxidized into the crotonic acid when exposed to air. At present, the main test method of the crotonic acid is a gas chromatography, the content of the crotonic acid is measured by a high performance liquid chromatography, and the detection of the crotonic acid in the food contact material is regulated by the entry-exit inspection and quarantine sweat industry standard SN/T5155-2019.
Although the limited amount is not specified in the country and related industries, the risk of crotonic acid is very clear. The state and the related industries do not establish official detection standards for detecting the substances in the cosmetics to detect the substances, and do not see related patents and paper reports; the detection limit is high in the prior art, and the method is limited in a laboratory and difficult to popularize.
SUMMERY OF THE UTILITY MODEL
In view of the above, the present invention has been made to provide a detection apparatus for measuring the content of crotonic acid in a cosmetic, which overcomes or at least partially solves the above problems.
In order to solve the above problem, the utility model discloses a detection device of crotonic acid content in survey cosmetics specifically can include: the device comprises a sampling mechanism, a preprocessing mechanism, a measuring mechanism and a data processing mechanism;
the sampling mechanism comprises a sampling scale with the precision of 0.0001 g;
the pretreatment mechanism comprises a colorimetric tube with a plug, a vortex oscillator, an ultrasonic extractor and a filter;
the colorimetric tube container with the plug is at least 10 mL;
the colorimetric tube with the plug for containing the ethyl alcohol solution of the methyl crotonate is placed in the oscillating part of the vortex oscillator;
placing the mixed solution subjected to vortex oscillation by a vortex oscillator in an extraction container of an ultrasonic extractor, wherein the mixed solution is an ethanol solution of the methyl crotonate;
the container before filtration of the filter is filled with the extracting solution obtained by the ultrasonic extraction instrument,
the filtered filtrate is filled into the filtered container of the filter;
a chromatographic column is arranged in the measuring mechanism and used for placing and testing the extracting solution;
the chromatographic column is filled with filtrate filtered by a filter;
the output end of the measuring mechanism is electrically connected to the data processing mechanism.
Further, the measuring mechanism is a high performance liquid chromatograph, and specifically comprises: high performance liquid chromatography-diode array detector.
Further, the data processing mechanism is a Computer device, and specifically may be a PC (Personal Computer) or a workstation or a server.
Further, the preprocessing mechanism further comprises: a centrifugal device with a centrifugal speed of at least 10000 r/min;
the centrifugal device is provided with a centrifugal container for placing the extracting solution;
a supernatant container for containing supernatant is arranged at the output position of the centrifugal device;
the filter is provided with a container for containing the supernatant.
Further, one sample to be weighed is a 0.2g sample.
Further, the measuring mechanism further includes:
the liquid phase pump, the sample inlet and the liquid phase detection assembly;
a sampling port of the liquid phase pump is connected to a container for containing the filtrate through a pipeline, and an output port of the liquid phase pump is connected to the sample inlet through a pipeline;
the sample inlet is connected to a first end of a chromatographic column;
the second end of the chromatography column is connected to a liquid detection assembly;
the liquid phase detection assembly is electrically connected to the data processing mechanism.
Further, the high performance liquid chromatograph has a chromatographic column length of 150mm, an inner diameter of 4.6mm, and a particle size of: 35 μm;
the mobile phase parameters were: 0.17% formic acid, 90:10 methanol; flow rate parameters: 1.0 mL/min; detection wavelength: 210 nm; column temperature: 30 ℃; sample introduction amount: 20 μ L run time: and (5) 12 min.
Further, the data processing mechanism further comprises a data output device;
the data output device is a printer and/or a drawing instrument and/or a memory.
The utility model discloses a following advantage: aiming at the current market in China, no specific equipment and detection standard exist, the content of the crotonic acid in the cosmetics is detected, the blank of the national standard is filled, and although the limited amount of the crotonic acid is not specified by the country and related industries, the dangerousness of the crotonic acid is very clear. The state and related industries do not establish official standards for detecting the substance in cosmetics, and related patents and papers are not reported. The utility model has low detection limit, the specific detection limit can reach 1mg/kg, the used equipment is easy to obtain, the use is simple, the detection is accurate, and the popularization is very good; recovery rates ranged from 80% to 110% by applying a standard recovery test to a typical cosmetic sample. Has good repeatability and reproducibility.
Drawings
FIG. 1 is a block diagram of the structure of a device for measuring the content of crotonic acid in cosmetics;
FIG. 2 is a chromatogram of the crotonic acid standard curve at each concentration point of the detection device for measuring crotonic acid content in cosmetic of the present invention;
fig. 3 is a high performance liquid chromatogram of a specific cosmetic sample according to an embodiment of the present invention.
The reference numerals are explained below:
1. a sampling mechanism; 2. a pretreatment mechanism; 3. a measuring mechanism; 4. a data processing mechanism; 21. a colorimetric cylinder with a plug; 22. a vortex oscillator; 23. an ultrasonic extractor; 24. a centrifugal device; 25. a filter; 31. a liquid phase pump; 32. a sample inlet; 33. a chromatographic column; 34. a liquid phase detection assembly; 41. a computer; 42. and (6) an output device.
Detailed Description
In order to make the above objects, features and advantages of the present invention more comprehensible, the present invention is described in detail with reference to the accompanying drawings and the detailed description.
One of the core ideas of the utility model lies in that, to on the present market of China, no specific equipment and detection standard, detect crotonic acid content in the cosmetics, fill the blank of national standard, although the country and relevant trade do not stipulate its limit of quantity, but crotonic acid be very clear and definite for danger. The state and related industries do not establish official standards for detecting the substance in cosmetics, and related patents and papers are not reported. The utility model discloses, it is low to detect the limit, and the concrete detection limit can reach 1mg/kg, and used equipment easily obtains, and is simple to use, detects the accuracy, has the generalizability.
Referring to fig. 1, a block diagram of a detection apparatus for determining crotonic acid content in cosmetics according to the present invention is shown, which may specifically include: the device comprises a sampling mechanism 1, a preprocessing mechanism 2, a measuring mechanism 3 and a data processing mechanism 4;
the sampling mechanism 1 comprises a sampling scale with the precision of 0.0001 g; the pretreatment mechanism 2 comprises a colorimetric tube with a plug 21, a vortex oscillator 22, an ultrasonic extractor 23 and a filter 25; the colorimetric tube container with the plug 21 is at least 10 mL; the colorimetric tube with a plug 21 for containing an ethanol solution of methyl crotonate is placed in the oscillating part of the vortex oscillator 22, wherein ethanol is arranged in the colorimetric tube with a plug 21, and a sample weighed by the sampling scale forms the ethanol solution of methyl crotonate; placing the mixed solution subjected to vortex oscillation by a vortex oscillator 22 in an extraction container of an ultrasonic extractor 23, wherein the mixed solution is an ethanol solution of the methyl crotonate; the extracting solution obtained by the ultrasonic extractor 23 is filled in the container before filtering of the filter 25, and the filtered filtrate is filled in the container after filtering of the filter 25; a chromatographic column 33 is arranged in the measuring mechanism 3, and the chromatographic column 33 is used for placing and testing the extracting solution; the chromatographic column 33 is filled with filtrate filtered by the filter 25; the output end of the measuring mechanism 3 is electrically connected to the data processing mechanism 4.
In another embodiment, the measuring mechanism 3 is a high performance liquid chromatograph, and specifically includes: high performance liquid chromatography-diode array detector.
In another embodiment, the data processing mechanism 4 is a Computer 41 device, which may be a PC (Personal Computer 41) or a workstation or a server.
In another embodiment, the preprocessing mechanism 2 further comprises: a centrifugal device 24 with a centrifugal speed of at least 10000 r/min; placing the extracting solution in a centrifugal container of the centrifugal device 24;
a supernatant container for containing supernatant is arranged at the output position of the centrifugal device 24, wherein the supernatant is liquid obtained by centrifuging the extracting solution for at least 5 minutes by the centrifugal device 24; the filter 25 has a container for containing the supernatant in the supernatant container.
In another embodiment, the weighed sample is a 0.2g sample.
In another embodiment, the measuring mechanism 3 further includes: a liquid phase pump 31, a sample inlet 32 and a liquid phase detection assembly 34;
a sampling port of the liquid phase pump 31 is connected to a container containing the filtrate through a pipeline, and an output port of the liquid phase pump 31 is connected to the sample inlet 32 through a pipeline; the sample inlet 32 is connected to a first end of a chromatography column 33; a second end of the chromatography column 33 is connected to a liquid detection assembly 34; the liquid phase detection assembly 34 is electrically connected to the data processing mechanism 4.
In another embodiment, the high performance liquid chromatograph has a column 33 having a length of 150mm, an inner diameter of 4.6mm, and a particle size of: 35 μm; the mobile phase parameters were: 0.17% formic acid, 90:10 methanol; flow rate parameters: 1.0 mL/min; detection wavelength: 210 nm; column temperature: 30 ℃; sample introduction amount: 20 μ L run time: 12 min;
referring to fig. 2, a crotonic acid standard substance curve is shown;
the standard curve linear range is given in the following table:
wherein the target substance retention time: crotonic acid 8.94 minutes.
As shown in FIG. 3, the method is characterized by high-performance liquid chromatography data of a certain cosmetic sample, high-performance separation, stable baseline and the like.
In another embodiment, the data processing mechanism 4 further comprises a data output device 42; the data output device 42 is a printer and/or a drawing instrument and/or a memory.
Finally, it should also be noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or terminal that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or terminal. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in a process, method, article, or terminal that comprises the element.
The above detailed description is made on the detection device for measuring the content of crotonic acid in cosmetics provided by the present invention, and the specific examples are applied herein to explain the principle and the implementation of the present invention, and the description of the above examples is only used to help understand the method and the core idea of the present invention; meanwhile, for the general technical personnel in the field, according to the idea of the present invention, there are changes in the specific implementation and application scope, to sum up, the content of the present specification should not be understood as the limitation of the present invention.
Claims (6)
1. A detection device for measuring the content of crotonic acid in cosmetics is characterized by comprising: the device comprises a sampling mechanism, a preprocessing mechanism, a measuring mechanism and a data processing mechanism;
the sampling mechanism comprises a sampling scale with the precision of 0.0001 g;
the pretreatment mechanism comprises a colorimetric tube with a plug, a vortex oscillator, an ultrasonic extractor and a filter;
the colorimetric tube container with the plug is at least 10 mL;
the colorimetric tube with the plug for containing the ethyl alcohol solution of the methyl crotonate is placed in the oscillating part of the vortex oscillator;
placing the mixed solution subjected to vortex oscillation by a vortex oscillator in an extraction container of an ultrasonic extractor, wherein the mixed solution is an ethanol solution of the methyl crotonate;
the container before filtration of the filter is filled with the extracting solution obtained by the ultrasonic extraction instrument,
the filtered filtrate is filled into the filtered container of the filter;
a chromatographic column is arranged in the measuring mechanism;
the chromatographic column is filled with filtrate filtered by a filter;
the output end of the measuring mechanism is electrically connected to the data processing mechanism.
2. The detection apparatus according to claim 1, wherein the measuring mechanism is a high performance liquid chromatograph, and specifically: high performance liquid chromatography-diode array detector.
3. The detection apparatus according to claim 2, wherein the data processing mechanism is a computer device, in particular a PC or a workstation or a server.
4. The testing device of claim 1, wherein said preprocessing mechanism further comprises: a centrifugal device with a centrifugal speed of at least 10000 r/min;
the centrifugal device is provided with a centrifugal container for placing the extracting solution;
a supernatant container for containing supernatant is arranged at the output position of the centrifugal device;
the filter is provided with a container for containing the supernatant.
5. The detection device of claim 2, wherein the measurement mechanism further comprises:
the liquid phase pump, the sample inlet and the liquid phase detection assembly;
a sampling port of the liquid phase pump is connected to a container for containing the filtrate through a pipeline, and an output port of the liquid phase pump is connected to the sample inlet through a pipeline;
the sample inlet is connected to a first end of a chromatographic column;
the second end of the chromatography column is connected to a liquid detection assembly;
the liquid phase detection assembly is electrically connected to the data processing mechanism.
6. The detection apparatus according to claim 3, wherein the data processing mechanism further comprises a data output device;
the data output device is a printer and/or a drawing instrument and/or a memory.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202021821583.1U CN215005145U (en) | 2020-08-26 | 2020-08-26 | Detection apparatus for crotonic acid content in survey cosmetics |
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| CN202021821583.1U CN215005145U (en) | 2020-08-26 | 2020-08-26 | Detection apparatus for crotonic acid content in survey cosmetics |
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