A test paper card for detecting boric acid and or borate in cosmetics and a detection method

Abstract

The application relates to the technical field of cosmetic detection, and particularly discloses a test paper card for detecting boric acid and / or borate in cosmetics and a detection method. The test paper card for detecting boric acid and / or borate in cosmetics comprises an activated sample pad, a functional reaction film and a PVC bottom plate which are sequentially attached, the activated sample pad is a glass fiber membrane soaked by a pretreatment reagent, the functional reaction film is a nitrocellulose membrane coated by a chromogenic reagent, the functional reaction film comprises an attaching area and a chromogenic area, the activated sample pad is located in the attaching area, and the chromogenic area is exposed to the environment. The application can be used for detecting whether boric acid and / or borate is contained in cosmetics, and can improve the sensitivity and stability of the detection of boric acid and / or borate in cosmetics.

Description

Technical Field

[0001] This invention relates to the technical field of cosmetic testing, and in particular to a test strip and testing method for boric acid and / or borates in cosmetics. Background Technology

[0002] Boric acid and its borates possess antibacterial, preservative, and pH-stabilizing properties; however, due to their well-established reproductive and developmental toxicity, potential cumulative skin irritation, and sensitization, their use in cosmetics is strictly limited by major regulatory agencies worldwide. China's "Cosmetic Safety Technical Specifications" (2015 edition) stipulates that boric acid and its borates can only be used in extremely low amounts (≤0.1% boric acid) in specific product categories, and explicitly prohibits their use in skincare products and talcum powders intended for children under three years of age. However, the high complexity of cosmetic matrices presents a significant challenge to the specific detection of boric acid.

[0003] In related technologies, a method for detecting boric acid and / or borates is disclosed, comprising the following steps: dissolving anhydrous acid in anhydrous protonated solvent to form reagent A; dissolving curcumin in anhydrous protonated solvent, then immersing it in filter paper, removing it and drying it to obtain turmeric test paper; mixing the sample to be tested with reagent A to obtain a mixture, adding the mixture dropwise onto the turmeric test paper, and qualitatively detecting boric acid and / or borates based on the color change of the turmeric test paper.

[0004] However, because oils, emulsifiers, and pigments in cosmetics can easily interfere with colorimetric analysis, leading to false positives or false negatives, the above detection methods will result in decreased detection sensitivity and stability when used to detect boric acid and / or borates in cosmetics. Summary of the Invention

[0005] To improve the sensitivity and stability of detecting boric acid and / or borates in cosmetics, this application provides a test strip and detection method for boric acid and / or borates in cosmetics.

[0006] In the first aspect, the test strip card for detecting boric acid and / or borates in cosmetics provided in this application adopts the following technical solution:

[0007] A test strip for detecting boric acid and / or borates in cosmetics includes an activated sample pad, a functionalized reaction membrane, and a PVC base plate sequentially bonded together. The activated sample pad is a glass fiber membrane pretreated with a pretreatment reagent, and the functionalized reaction membrane is a nitrocellulose membrane coated with a colorimetric reagent. The functionalized reaction membrane includes a bonding area and a colorimetric area, with the activated sample pad located in the bonding area and the colorimetric area exposed to the environment.

[0008] By employing the above technical solution, the sample to be tested is dropped onto an activated sample pad. After penetrating the activated sample pad, the sample reacts with the color-developing components of the functionalized reaction membrane, causing a color change in the membrane. This allows for the determination of whether the sample contains boric acid and / or borates. The activated sample pad filters interfering components from the sample, helping to reduce the impact of interfering components in cosmetics on the detection results. After penetrating the activated sample pad, the sample seeps into the bonding area and reacts with the color-developing components on the functionalized reaction membrane, causing both the bonding and color-developing areas of the membrane to change color. Since the color-developing area is exposed to the environment, the detection result can be quickly obtained by observing it. Furthermore, the content of boric acid and / or borates can be determined based on the depth of the color, enabling rapid detection and improving the sensitivity and stability of the assay.

[0009] In one specific implementation, a colorimetric card is also attached to the PVC base plate.

[0010] By adopting the above technical solution, once the color change stabilizes, it can be compared with a colorimetric card. Based on the depth of color, the content of boric acid and / or borate can be determined, making it easy to quickly obtain the test results.

[0011] In one specific implementation scheme, the pretreatment reagent comprises the following raw materials by weight: 40-60 parts alkyl glycoside, 130-170 parts triethyl orthoformate, 180-250 parts cyclohexanediol dicarboxylate, 90-130 parts camphor sulfonic acid, 45-60 parts polyethylene glycol 400, and the balance being anhydrous ethanol, totaling 1000 parts.

[0012] By employing the above technical solution and with the aforementioned raw material ratio, alkyl glycosides cleave the cosmetic oil-water interface film, releasing embedded boric acid. Cyclohexanedimethyl dicarboxylate selectively dissolves boric acid molecules, filtering pigment / colloidal particles. Triethyl orthoformate reacts with water to produce ethanol and formate, which can quickly remove water without interfering with color development. Camphor sulfonic acid provides the acidic environment required for color development and has a high boiling point, making it non-volatile at room temperature, thus helping to extend the shelf life of the test strips. The synergistic effect of triethyl orthoformate and camphor sulfonic acid can also create a localized superacid environment in the pores of the glass fiber membrane, helping to lower the activation energy of boric acid and increase the reaction rate between boric acid and the color-developing components, thereby improving the color development sensitivity. Polyethylene glycol 400 can slow down the diffusion rate of reactants, ensuring thorough impurity removal, while anhydrous ethanol, as a solvent with low water content, can reduce the interference of water on color development.

[0013] In one specific implementation, the pretreatment reagent further includes the following raw materials in parts by weight: 25-35 parts bentonite and 15-25 parts hexadecyltrimethylammonium bromide.

[0014] By adopting the above technical solution, hexadecyltrimethylammonium bromide can provide cation adsorption sites, and the interlayer spacing of bentonite can accommodate boric acid molecules but not oils. Therefore, the synergistic effect of bentonite and hexadecyltrimethylammonium bromide can selectively adsorb oils, pigments, and colloidal particles, further reducing the interference of interfering components in cosmetics on the detection results and improving the sensitivity and stability of the test strip.

[0015] In one specific implementation, the pretreatment reagent further includes silanized silica.

[0016] By employing the above technical solution, silanized silica can undergo silanization crosslinking, thereby deactivating silicone oil, reducing system viscosity, and precipitating boric acid encapsulated in silicone oil. It can also synergistically remove impurities with bentonite, thus further improving the sensitivity and stability of test strips.

[0017] In one specific implementation scheme, the colorimetric reagent comprises the following raw materials in parts by weight, based on the total weight of the colorimetric reagent: 0.8-1.5 parts curcumin, 25-35 parts polyethylene glycol 6000, 90-120 parts zinc 2-nitrobenzenesulfonate, 450-550 parts silica aerogel powder, 40-60 parts polyether-modified siloxane, with the balance being ethyl acetate, totaling 1000 parts.

[0018] By employing the above technical solution, curcumin is the main component of the colorimetric reaction. Polyethylene glycol 6000 and silica aerogel powder can encapsulate curcumin, which can improve the thermal stability of curcumin and isolate cosmetic residues, thereby improving the colorimetric stability. Zinc 2-nitrobenzenesulfonate can decompose in situ to produce sulfonic acid, maintaining an acidic detection environment. Polyether-modified siloxane helps improve the permeability and leveling of the liquid, resulting in more uniform color development. Ethyl acetate is a fast-evaporating solvent, facilitating the curing of the colorimetric reagent.

[0019] In one specific implementation, the colorimetric reagent further includes the following raw material in parts by weight: 30-50 parts ammonium molybdate.

[0020] By employing the above technical solution, ammonium molybdate and zinc 2-nitrobenzenesulfonate can synergistically maintain a high colorimetric efficiency detection environment in a strongly acidic environment. Furthermore, it can synergistically work with polyethylene glycol 6000 to prevent the hydrolytic deactivation of heteropolyacids, improve catalytic stability, thereby accelerating color development and enhancing colorimetric stability.

[0021] Secondly, this application provides a method for detecting boric acid and / or borates in cosmetics, which adopts the following technical solution:

[0022] A method for detecting boric acid and / or borates in cosmetics, comprising the following steps:

[0023] S1. Mix alkyl glycoside, triethyl orthoformate, cyclohexanedimethyl dimethyl ester, camphor sulfonic acid, polyethylene glycol 400 and anhydrous ethanol evenly according to the proportion to obtain a pretreatment reagent. Immerse the glass fiber membrane in the pretreatment layer solution, take it out, and dry it to obtain an activated sample pad.

[0024] S2. According to the proportion, curcumin, polyethylene glycol 6000, zinc 2-nitrobenzenesulfonate, silica aerogel powder, polyether-modified siloxane and ethyl acetate are mixed evenly to obtain a colorimetric reagent. The colorimetric reagent is coated on the surface of nitrocellulose membrane and cured to obtain a functionalized reaction membrane.

[0025] S3. The functionalized reactive membrane is bonded to a PVC substrate. The surface of the functionalized reactive membrane is divided into a bonding area and a color development area. The activated sample pad is bonded to the bonding area of ​​the functionalized reactive membrane, and the color development area is exposed to the environment to obtain the test strip card.

[0026] S4. Dissolve the cosmetic to be tested in deionized water, centrifuge, and collect the lower clear liquid.

[0027] S5. Add the lower clear liquid droplet to the surface of the activated sample pad on the test strip, let it stand for 25-30 seconds, and observe the color change of the functionalized reaction membrane to perform qualitative detection of boric acid and / or borate.

[0028] In one specific feasible implementation, in step S3: the functionalized reactive membrane and the colorimetric card are both bonded to a PVC substrate, the surface of the functionalized reactive membrane is divided into a bonding area and a color development area, the activated sample pad is bonded to the bonding area of ​​the functionalized reactive membrane, and the color development area is exposed to the environment to obtain the test strip card.

[0029] In a specific feasible implementation, in step S5: the lower clear liquid is dropped onto the surface of the activated sample pad of the test strip card, left to stand for 25-30 seconds, and the final color development of the functionalized reaction membrane is observed. The color of the functionalized reaction membrane is compared with the colorimetric card. Based on the final color development of the functionalized reaction membrane, it is determined whether the cosmetic to be tested contains boric acid and / or borates, and the level of boric acid and / or borates in the cosmetic to be tested.

[0030] By adopting the above technical solution and test strip, and by pre-centrifuging the cosmetic to be tested to remove impurities, the test results can be obtained quickly at room temperature without heating, reducing the influence of interfering components in the cosmetic, and color development only requires 25-30 seconds. Therefore, the detection method of this application has excellent sensitivity and stability.

[0031] In summary, this application has the following beneficial effects:

[0032] 1. This application can be used to detect whether cosmetics contain boric acid and / or borates, and can improve the sensitivity and stability of detecting boric acid and / or borates in cosmetics.

[0033] 2. In this application, pretreatment reagents and colorimetric reagents with specific raw material ratios are preferred, which can reduce the interference of interfering components in cosmetics on the test results and further improve the sensitivity and stability of the test strip.

[0034] 3. The method of this application can quickly obtain the test results at room temperature without heating, which reduces the influence of interfering ingredients in cosmetics and has excellent sensitivity and stability. Attached Figure Description

[0035] Figure 1 This is a schematic diagram of the structure of the test strip card for detecting boric acid and / or borates in cosmetics in Example 1 of this application;

[0036] Figure 2 This is a schematic diagram of the structure of the functionalized reactive membrane in Example 1 of this application;

[0037] Figure 3 This is a schematic diagram of the structure of the test strip card for detecting boric acid and / or borates in cosmetics in Example 16 of this application;

[0038] Figure 4 Images of the colorimetric card used in Embodiment 16 of this application and the performance testing experiment;

[0039] Figure labels: 1. Activated sample pad; 2. Functionalized reaction membrane; 21. Adhesion area; 22. Color development area; 3. PVC base plate; 4. Colorimetric card. Detailed Implementation

[0040] Unless otherwise specified, all raw materials used in the embodiments and comparative examples of this application were commercially available. The glass fiber membrane was a Thermo Fisher Scientific D28 glass cellulose filter membrane. The nitrocellulose membrane was purchased from Suzhou Caishi Instrument Co., Ltd., with a thickness of 0.1 mm, a monofilament diameter of 0.1 mm, and a molecular weight cutoff of 5 kDa. The PVC substrate was a DB-6 type PVC substrate purchased from Shanghai Jieyi Biotechnology Co., Ltd. The alkyl glycoside was purchased from Shanghai Fakai Chemical Co., Ltd., specification APG0810. Triethyl orthoformate was purchased from Nanjing Chemical Reagent Co., Ltd., purity AR grade. Cyclohexanediol dicarboxylate was purchased from Suzhou Senfida Chemical Co., Ltd., purity AR grade. Camphor sulfonic acid was dextrorotatory camphor sulfonic acid purchased from Hubei Maidehao Biotechnology Co., Ltd., purity AR grade. Polyethylene glycol 400 and polyethylene glycol 6000 were both purchased from Shandong Baihua Chemical Co., Ltd., purity AR grade. Curcumin was purchased from Chengdu Purifa Technology Development Co., Ltd. as bisdemethoxycurcumin, with a purity of AR grade. Zinc 2-nitrobenzenesulfonate was purchased from Jinjinle (Hunan) Chemical Co., Ltd., with a purity of AR grade. Silica aerogel powder was purchased from Suzhou Zhongcui Nanomaterials Technology Co., Ltd. Polyether-modified siloxane was purchased from Wuhan Shuer Biotechnology Co., Ltd. as H-408 type polyether-modified siloxane. Ethyl acetate was purchased from Foshan Changxing New Materials Co., Ltd., with a purity of AR grade. Bentonite was purchased from Zhejiang Fenghong New Materials Co., Ltd. Hexadecyltrimethylammonium bromide was purchased from Shanghai Yifengda Chemical Technology Co., Ltd., with a purity of AR grade. The nano-fumed silica was AEROSIL R 812. Trimethylchlorosilane was purchased from Changzhou Guangcheng Chemical Co., Ltd., with a purity of AR grade. Ammonium molybdate was purchased from Henan Mingzhixin Chemical Products Co., Ltd., with a purity of AR grade.

[0041] The present application will be further described in detail below with reference to embodiments and comparative examples.

[0042] Example

[0043] Example 1

[0044] like Figure 1 and Figure 2 As shown, this embodiment provides a test strip for detecting boric acid and / or borates in cosmetics, comprising, from top to bottom, an activated sample pad 1, a functionalized reaction membrane 2, and a PVC base plate 3. The activated sample pad 1 is a glass fiber membrane pretreated with a pretreatment reagent, and the functionalized reaction membrane 2 is a nitrocellulose membrane coated with a colorimetric reagent.

[0045] The pretreatment reagents include the following raw materials: 50g alkyl glycoside, 150g triethyl orthoformate, 215g cyclohexanedimethyl dimethyl ester, 110g camphor sulfonic acid, 52g polyethylene glycol 400, and the balance being anhydrous ethanol, totaling 1000g.

[0046] The colorimetric reagent consists of the following raw materials: 1.2g curcumin, 30g polyethylene glycol 6000, 105g zinc 2-nitrobenzenesulfonate, 500g silica aerogel powder, 50g polyether-modified siloxane, and the balance being ethyl acetate, totaling 1000g.

[0047] This embodiment also provides a method for detecting boric acid and / or borates in cosmetics, comprising the following steps:

[0048] S1. According to the above proportions, mix alkyl glycoside, triethyl orthoformate, cyclohexanedimethyl dicarboxylate, camphor sulfonic acid, polyethylene glycol 400, and anhydrous ethanol, and stir until homogeneous to obtain the pretreatment reagent. Completely immerse the glass fiber membrane in the pretreatment solution, soak for 12 minutes, then remove the glass fiber membrane and air dry at 40°C to obtain activated sample pad 1.

[0049] S2. According to the above proportions, curcumin, polyethylene glycol 6000, zinc 2-nitrobenzenesulfonate, silica aerogel powder, polyether-modified siloxane, and ethyl acetate are mixed and stirred until homogeneous to obtain a colorimetric reagent. Then, the colorimetric reagent is coated on the upper surface of the nitrocellulose membrane and allowed to stand at -20°C for 25 hours to obtain functionalized reaction membrane 2.

[0050] S3. The functionalized reaction membrane 2 is attached to the PVC base plate 3 with the surface coated with the colorimetric reagent facing upward. The surface of the functionalized reaction membrane 2 is divided into an attachment area 21 and a colorimetric area 22. The activated sample pad 1 is then attached to the attachment area 21 of the functionalized reaction membrane 2, and the colorimetric area 22 is exposed to the environment to obtain the test strip card.

[0051] S4. Dissolve the cosmetic product to be tested in deionized water at a weight-to-volume ratio of 0.2 g / mL, centrifuge at 3000 rpm for 3.5 minutes, and collect the lower clear liquid.

[0052] S5. Take 50 μL of the lower supernatant and drop it onto the surface of the activated sample pad 1 of the test paper. Let it stand for 25 seconds and observe the color change of the functionalized reaction membrane 2 to perform qualitative detection of boric acid and / or borates.

[0053] Example 2

[0054] The only difference between this embodiment and Example 1 is that the pretreatment reagent includes the following raw materials: 40g alkyl glycoside, 130g triethyl orthoformate, 180g cyclohexanedimethyl dimethyl ester, 90g camphor sulfonic acid, 45g polyethylene glycol 400, and the balance is anhydrous ethanol, totaling 1000g.

[0055] Example 3

[0056] The only difference between this embodiment and Example 1 is that the pretreatment reagent includes the following raw materials: 60g alkyl glycoside, 170g triethyl orthoformate, 250g cyclohexanedimethyl dimethyl ester, 130g camphor sulfonic acid, 60g polyethylene glycol 400, and the balance is anhydrous ethanol, totaling 1000g.

[0057] Example 4

[0058] The only difference between this embodiment and Example 1 is that the colorimetric reagent includes the following raw materials: 0.8g curcumin, 25g polyethylene glycol 6000, 90g zinc 2-nitrobenzenesulfonate, 450g silica aerogel powder, 40g polyether-modified siloxane, and the balance being ethyl acetate, totaling 1000g.

[0059] Example 5

[0060] The only difference between this embodiment and Example 1 is that the colorimetric reagent includes the following raw materials: 1.5g curcumin, 35g polyethylene glycol 6000, 120g zinc 2-nitrobenzenesulfonate, 550g silica aerogel powder, 60g polyether-modified siloxane, and the balance being ethyl acetate, totaling 1000g.

[0061] Example 6

[0062] The difference between this embodiment and Example 1 is that the pretreatment reagent includes the following raw materials: 50g alkyl glycoside, 150g triethyl orthoformate, 215g cyclohexanediol dicarboxylate, 110g camphor sulfonic acid, 52g polyethylene glycol 400, 25g bentonite, 15g hexadecyltrimethylammonium bromide, and the balance is anhydrous ethanol, totaling 1000g. In the method for detecting boric acid and / or borates in cosmetics, step S1 is as follows: Alkyl glycoside, triethyl orthoformate, cyclohexanediol dicarboxylate, camphor sulfonic acid, polyethylene glycol 400, bentonite, hexadecyltrimethylammonium bromide, and anhydrous ethanol are mixed according to the above proportions and stirred until homogeneous to obtain the pretreatment reagent. The glass fiber membrane is completely immersed in the pretreatment layer solution for 12 minutes. After immersion, the glass fiber membrane is removed and dried in a ventilated environment at 40°C to obtain the activated sample pad.

[0063] Example 7

[0064] The difference between this embodiment and Example 1 is that the pretreatment reagent includes the following raw materials: 50g alkyl glycoside, 150g triethyl orthoformate, 215g cyclohexanediol dicarboxylate, 110g camphor sulfonic acid, 52g polyethylene glycol 400, 30g bentonite, 20g hexadecyltrimethylammonium bromide, and the balance being anhydrous ethanol, totaling 1000g. In the method for detecting boric acid and / or borates in cosmetics, step S1 is as follows: Alkyl glycoside, triethyl orthoformate, cyclohexanediol dicarboxylate, camphor sulfonic acid, polyethylene glycol 400, bentonite, hexadecyltrimethylammonium bromide, and anhydrous ethanol are mixed according to the above proportions and stirred until homogeneous to obtain the pretreatment reagent. The glass fiber membrane is completely immersed in the pretreatment layer solution for 12 minutes. After immersion, the glass fiber membrane is removed and dried in a ventilated environment at 40°C to obtain the activated sample pad.

[0065] Example 8

[0066] The difference between this embodiment and Example 1 is that the pretreatment reagent includes the following raw materials: 50g alkyl glycoside, 150g triethyl orthoformate, 215g cyclohexanediol dicarboxylate, 110g camphor sulfonic acid, 52g polyethylene glycol 400, 35g bentonite, 25g hexadecyltrimethylammonium bromide, and the balance being anhydrous ethanol, totaling 1000g. In the method for detecting boric acid and / or borates in cosmetics, step S1 is as follows: Alkyl glycoside, triethyl orthoformate, cyclohexanediol dicarboxylate, camphor sulfonic acid, polyethylene glycol 400, bentonite, hexadecyltrimethylammonium bromide, and anhydrous ethanol are mixed according to the above proportions and stirred until homogeneous to obtain the pretreatment reagent. The glass fiber membrane is completely immersed in the pretreatment layer solution for 12 minutes. After immersion, the glass fiber membrane is removed and dried in a ventilated environment at 40°C to obtain the activated sample pad.

[0067] Example 9

[0068] The difference between this embodiment and Example 1 is that the pretreatment reagent includes the following raw materials: 50g alkyl glycoside, 150g triethyl orthoformate, 215g cyclohexanediol dicarboxylate, 110g camphor sulfonic acid, 52g polyethylene glycol 400, 30g bentonite, 20g hexadecyltrimethylammonium bromide, 20g silanized silica, and the balance being anhydrous ethanol, totaling 1000g. In the method for detecting boric acid and / or borates in cosmetics, step S1 is as follows: Alkyl glycoside, triethyl orthoformate, cyclohexanediol dicarboxylate, camphor sulfonic acid, polyethylene glycol 400, bentonite, hexadecyltrimethylammonium bromide, silanized silica, and anhydrous ethanol are mixed according to the above proportions and stirred until homogeneous to obtain the pretreatment reagent. The glass fiber membrane is completely immersed in the pretreatment layer solution for 12 minutes. After immersion, the glass fiber membrane is removed and dried in a ventilated environment at 40°C to obtain the activated sample pad.

[0069] The silanized silica was prepared by the following steps: nano-sized fumed silica was mixed with trimethylchlorosilane at a weight percentage of 2 g / mL, heated to 70°C, and kept at that temperature for 6 h. The mixture was then filtered, and the filtered solid was washed three times alternately with anhydrous toluene and anhydrous ethanol. The solid was then dried at 60°C for 12 h to obtain silanized silica.

[0070] Example 10

[0071] The difference between this embodiment and Example 1 lies only in that the colorimetric reagent comprises the following raw materials: 1.2g curcumin, 30g polyethylene glycol 6000, 105g zinc 2-nitrobenzenesulfonate, 500g silica aerogel powder, 50g polyether-modified siloxane, 30g ammonium molybdate, and the balance being ethyl acetate, totaling 1000g. In the method for detecting boric acid and / or borates in cosmetics, step S2 is as follows: Curcumin, polyethylene glycol 6000, zinc 2-nitrobenzenesulfonate, silica aerogel powder, polyether-modified siloxane, ammonium molybdate, and ethyl acetate are mixed according to the above proportions and stirred until homogeneous to obtain the colorimetric reagent. Then, the colorimetric reagent is coated onto the upper surface of a nitrocellulose membrane and allowed to stand at -20°C for 25 hours to obtain a functionalized reaction membrane.

[0072] Example 11

[0073] The difference between this embodiment and Example 1 lies only in that the colorimetric reagent comprises the following raw materials: 1.2g curcumin, 30g polyethylene glycol 6000, 105g zinc 2-nitrobenzenesulfonate, 500g silica aerogel powder, 50g polyether-modified siloxane, 40g ammonium molybdate, and the balance being ethyl acetate, totaling 1000g. In the method for detecting boric acid and / or borates in cosmetics, step S2 is as follows: Curcumin, polyethylene glycol 6000, zinc 2-nitrobenzenesulfonate, silica aerogel powder, polyether-modified siloxane, ammonium molybdate, and ethyl acetate are mixed according to the above proportions and stirred until homogeneous to obtain the colorimetric reagent. Then, the colorimetric reagent is coated onto the upper surface of a nitrocellulose membrane and allowed to stand at -20°C for 25 hours to obtain a functionalized reaction membrane.

[0074] Example 12

[0075] The difference between this embodiment and Example 1 lies only in that the colorimetric reagent comprises the following raw materials: 1.2g curcumin, 30g polyethylene glycol 6000, 105g zinc 2-nitrobenzenesulfonate, 500g silica aerogel powder, 50g polyether-modified siloxane, 50g ammonium molybdate, and the balance being ethyl acetate, totaling 1000g. In the method for detecting boric acid and / or borates in cosmetics, step S2 is as follows: Curcumin, polyethylene glycol 6000, zinc 2-nitrobenzenesulfonate, silica aerogel powder, polyether-modified siloxane, ammonium molybdate, and ethyl acetate are mixed according to the above proportions and stirred until homogeneous to obtain the colorimetric reagent. Then, the colorimetric reagent is coated onto the upper surface of a nitrocellulose membrane and allowed to stand at -20°C for 25 hours to obtain a functionalized reaction membrane.

[0076] Example 13

[0077] The only difference between this embodiment and Example 1 is that the pretreatment reagent includes the following raw materials: 50g alkyl glycoside, 150g triethyl orthoformate, 215g cyclohexanedimethyl dimethyl ester, 110g camphor sulfonic acid, 52g polyethylene glycol 400, 30g bentonite, 20g cetyltrimethylammonium bromide, 20g silanized silica, and the balance being anhydrous ethanol, totaling 1000g.

[0078] The colorimetric reagent consists of the following raw materials: 1.2g curcumin, 30g polyethylene glycol 6000, 105g zinc 2-nitrobenzenesulfonate, 500g silica aerogel powder, 50g polyether-modified siloxane, 40g ammonium molybdate, and the balance being ethyl acetate, totaling 1000g.

[0079] In the method for detecting boric acid and / or borates in cosmetics, step S1 is as follows: Alkyl glycoside, triethyl orthoformate, cyclohexanedimethyl dicarboxylate, camphor sulfonic acid, polyethylene glycol 400, bentonite, hexadecyltrimethylammonium bromide, silanized silica, and anhydrous ethanol are mixed in the above proportions and stirred until homogeneous to obtain the pretreatment reagent. The glass fiber membrane is completely immersed in the pretreatment solution for 12 minutes. After immersion, the glass fiber membrane is removed and dried in a ventilated environment at 40°C to obtain the activated sample pad.

[0080] Step S2 is as follows: According to the above proportions, curcumin, polyethylene glycol 6000, zinc 2-nitrobenzenesulfonate, silica aerogel powder, polyether-modified siloxane, ammonium molybdate, and ethyl acetate are mixed and stirred until homogeneous to obtain a colorimetric reagent. Then, the colorimetric reagent is coated onto the upper surface of a nitrocellulose membrane and allowed to stand at -20°C for 25 hours to obtain a functionalized reaction membrane.

[0081] The silanized silica was prepared by the following steps: nano-sized fumed silica was mixed with trimethylchlorosilane at a weight percentage of 2 g / mL, heated to 70°C, and kept at that temperature for 6 h. The mixture was then filtered, and the filtered solid was washed three times alternately with anhydrous toluene and anhydrous ethanol. The solid was then dried at 60°C for 12 h to obtain silanized silica.

[0082] Example 14

[0083] The only difference between this embodiment and Embodiment 1 is that step S5 is as follows: 50 μL of the lower supernatant is dropped onto the surface of the activated sample pad of the test paper, left to stand for 28 seconds, and the color change of the functionalized reaction membrane is observed to perform qualitative detection of boric acid and / or borates.

[0084] Example 15

[0085] The only difference between this embodiment and Embodiment 1 is that step S5 is as follows: 50 μL of the lower supernatant is dropped onto the surface of the activated sample pad of the test paper, left to stand for 30 seconds, and the color change of the functionalized reaction membrane is observed to perform qualitative detection of boric acid and / or borates.

[0086] Example 16

[0087] like Figure 3 and Figure 4 As shown, the only difference between this embodiment and Embodiment 1 is that the test strip for boric acid and / or borates in cosmetics includes, from top to bottom, an activated sample pad 1, a functionalized reaction membrane 2, and a PVC base plate 3. A colorimetric card 4 is also attached to the PVC base plate 3. The activated sample pad 1 is a glass fiber membrane that has been pretreated with a reagent, and the functionalized reaction membrane 2 is a nitrocellulose membrane that has been coated with a colorimetric reagent.

[0088] In the detection method of boric acid and / or borates in cosmetics, step S3 is as follows: both the functionalized reaction membrane 2 and the colorimetric card 4 are attached to the PVC base plate 3, with the surface of the functionalized reaction membrane 2 coated with the colorimetric reagent facing upwards. The surface of the functionalized reaction membrane 2 is divided into an attachment area 21 and a colorimetric area 22. The activated sample pad 1 is then attached to the attachment area 21 of the functionalized reaction membrane 2, and the colorimetric area 22 is exposed to the environment to obtain the test strip card.

[0089] Step S5 is as follows: Take 50 μL of the lower clear liquid and drop it onto the surface of the activated sample pad 1 of the test paper card. Let it stand for 25 seconds and observe the final color development of the functionalized reaction membrane 2. Compare the color of the functionalized reaction membrane 2 with the colorimetric card 4. Based on the final color development of the functionalized reaction membrane 2, determine whether the cosmetic to be tested contains boric acid and / or borates, and the level of boric acid and / or borates in the cosmetic to be tested.

[0090] Comparative Example

[0091] Comparative Example 1

[0092] The only difference between this comparative example and Example 1 is that the test strip for boric acid and / or borates in cosmetics includes a functionalized reactive membrane and a PVC base plate that are sequentially bonded from top to bottom.

[0093] Comparative Example 2

[0094] The only difference between this comparative example and Example 1 is that, in the test strip and detection method for boric acid and / or borates in cosmetics, the pretreatment reagent includes the following raw materials: 150g triethyl orthoformate, 215g cyclohexanedimethyl dimethyl ester, 110g camphor sulfonic acid, 52g polyethylene glycol 400, and the balance being anhydrous ethanol, totaling 1000g.

[0095] Comparative Example 3

[0096] The only difference between this comparative example and Example 1 is that, in the test strip and detection method for boric acid and / or borates in cosmetics, the pretreatment reagent includes the following raw materials: 50g alkyl glycoside, 215g cyclohexanedimethyl dicarboxylate, 110g camphor sulfonic acid, 52g polyethylene glycol 400, and the balance being anhydrous ethanol, totaling 1000g.

[0097] Comparative Example 4

[0098] The only difference between this comparative example and Example 1 is that, in the test strip and detection method for boric acid and / or borates in cosmetics, the pretreatment reagent includes the following raw materials: 50g alkyl glycoside, 150g triethyl orthoformate, 110g camphor sulfonic acid, 52g polyethylene glycol 400, and the balance being anhydrous ethanol, totaling 1000g.

[0099] Comparative Example 5

[0100] The only difference between this comparative example and Example 1 is that, in the test strip and detection method for boric acid and / or borates in cosmetics, the pretreatment reagent includes the following raw materials: 50g alkyl glycoside, 150g triethyl orthoformate, 215g cyclohexanedimethyl dimethyl ester, 52g polyethylene glycol 400, and the balance being anhydrous ethanol, totaling 1000g.

[0101] Comparative Example 6

[0102] The only difference between this comparative example and Example 1 is that, in the test strip and detection method for boric acid and / or borates in cosmetics, the pretreatment reagent includes the following raw materials: 50g alkyl glycoside, 150g triethyl orthoformate, 215g cyclohexanedimethyl dimethyl ester, 110g camphor sulfonic acid, and the balance being anhydrous ethanol, totaling 1000g.

[0103] Comparative Example 7

[0104] The only difference between this comparative example and Example 1 is that, in the test strip and detection method for boric acid and / or borates in cosmetics, the colorimetric reagent includes the following raw materials: 1.2g curcumin, 105g zinc 2-nitrobenzenesulfonate, 500g silica aerogel powder, 50g polyether-modified siloxane, and the balance being ethyl acetate, totaling 1000g.

[0105] Comparative Example 8

[0106] The only difference between this comparative example and Example 1 is that, in the test strip and detection method for boric acid and / or borates in cosmetics, the colorimetric reagent includes the following raw materials: 1.2g curcumin, 30g polyethylene glycol 6000, 500g silica aerogel powder, 50g polyether-modified siloxane, and the balance being ethyl acetate, totaling 1000g.

[0107] Comparative Example 9

[0108] The only difference between this comparative example and Example 1 is that, in the test strip and detection method for boric acid and / or borates in cosmetics, the colorimetric reagent includes the following raw materials: 1.2g curcumin, 30g polyethylene glycol 6000, 105g zinc 2-nitrobenzenesulfonate, 50g polyether-modified siloxane, and the balance being ethyl acetate, totaling 1000g.

[0109] Comparative Example 10

[0110] The only difference between this comparative example and Example 1 is that, in the test strip and detection method for boric acid and / or borates in cosmetics, the colorimetric reagent includes the following raw materials: 1.2g curcumin, 30g polyethylene glycol 6000, 105g zinc 2-nitrobenzenesulfonate, 500g silica aerogel powder, and the balance being ethyl acetate, totaling 1000g.

[0111] Performance testing

[0112] The following performance tests were performed on Examples 1-16 and Comparative Examples 1-10:

[0113] Preparation of the tested cosmetic: 14g stearic acid, 1.0g monoglyceride, 1g 1618 alcohol, 2g white oil, 8g glycerin, 0.5g potassium hydroxide, and 73.5g deionized water were mixed evenly to obtain a basic cream. Then, the basic cream, boric acid, and borate were mixed evenly to obtain the tested cosmetics with boric acid and borate contents of 0.5mg / kg, 5mg / kg, 100mg / kg, 1000mg / kg, 1100mg / kg, and 1200mg / kg, respectively.

[0114] As attached Figure 4 As shown, the color chart is divided into four categories according to color: bright yellow, dark yellow, orange-red, and deep red.

[0115] Example 1: Testing of cosmetics with different boric acid and borates: The test strips and methods for boric acid and / or borates in cosmetics described in Example 1 were used to test the cosmetics with different contents, with a basic cream as the control group. The final color was compared with the colorimetric card and recorded, as shown in Table 1.

[0116] Testing of the cosmetics in each embodiment and comparative example: The test strips and methods for boric acid and / or borates in the cosmetics of each embodiment and comparative example were used to test the cosmetics with boric acid and borates content of 5 mg / kg, 100 mg / kg, and 1000 mg / kg, respectively. Each cosmetic with boric acid and borates content was tested 5 times. The final color development of each cosmetic with boric acid and borates content was compared with the colorimetric card, and the final color development was recorded as shown in Table 2.

[0117] Table 1

[0118]

[0119]

[0120] Table 2

[0121]

[0122]

[0123] Referring to Example 1 and Table 1, when testing cosmetics using the test strips prepared in Example 1 of this application, if the final color of the test strip is bright yellow, it can be determined that the content of boric acid and borate in the cosmetic is ≤5 mg / kg. If the final color of the test strip is dark yellow, it can be determined that the content of boric acid and borate in the cosmetic is ≤100 mg / kg. If the final color of the test strip is orange-red, it can be determined that the content of boric acid and borate in the cosmetic is ≤1000 mg / kg. If the final color of the test strip is deep red, it can be determined that the content of boric acid and borate in the cosmetic is ≥1100 mg / kg.

[0124] Based on Example 1 and Comparative Examples 1-10, and in conjunction with Table 2, it can be seen that in Example 1, the test results for the cosmetics with boric acid and borate contents of 5 mg / kg and 100 mg / kg showed only one difference in color development, while the test results for the cosmetics with boric acid and borate contents of 1000 mg / kg were identical.

[0125] Comparative Examples 1-9 all showed 5 bright yellow results for the tested cosmetics with boric acid and borate content of 5 mg / kg. Comparative Example 10 showed 4 bright yellow results and 1 dark yellow result for the tested cosmetics with boric acid and borate content of 5 mg / kg. The test results for the tested cosmetics with boric acid and borate content of 100 mg / kg and 1000 mg / kg in Comparative Examples 1-10 were unstable, showing bright yellow, dark yellow, orange-red, and deep red hues. This indicates that the test strip and detection method of Example 1 have better stability. Furthermore, it is more sensitive to tested cosmetics with low boric acid and borate content, and the color development stabilizes after 25 seconds, indicating a fast detection speed.

[0126] As can be seen from Examples 1-16 and Table 2, the test results of the cosmetics to be tested with boric acid and borates of 5 mg / kg, 100 mg / kg and 1000 mg / kg in Examples 1-16 showed at most one different color development in each group. This indicates that the test strips and detection methods used in Examples 1-16 have excellent sensitivity and stability.

[0127] Furthermore, in Example 13, the color development results for the tested cosmetics with boric acid and borate contents of 5 mg / kg, 100 mg / kg, and 1000 mg / kg were identical in each of the five tests. This indicates that the test strip and detection method of Example 13 exhibit the best sensitivity and stability.

[0128] This specific embodiment is merely an explanation of this application and is not intended to limit it. After reading this specification, those skilled in the art can make modifications to this embodiment without contributing any inventive step, but such modifications are protected by patent law as long as they fall within the scope of the claims of this application.

Claims

1. A test strip for detecting boric acid and / or borates in cosmetics, characterized in that, The device includes an activated sample pad (1), a functionalized reaction membrane (2), and a PVC base plate (3) that are sequentially bonded together. The activated sample pad (1) is a glass fiber membrane that has been soaked in a pretreatment reagent. The functionalized reaction membrane (2) is a nitrocellulose membrane that has been coated with a colorimetric reagent. The functionalized reaction membrane (2) includes a bonding area (21) and a colorimetric area (22). The activated sample pad (1) is located in the bonding area (21), and the colorimetric area (22) is exposed to the environment. Based on the total weight of the pretreatment reagent, the pretreatment reagent comprises the following raw materials in parts by weight: 40-60 parts alkyl glycoside, 130-170 parts triethyl orthoformate, 180-250 parts cyclohexanediol dicarboxylate, 90-130 parts camphor sulfonic acid, 45-60 parts polyethylene glycol 400, and the balance being anhydrous ethanol, totaling 1000 parts. Based on the total weight of the colorimetric reagent, the colorimetric reagent comprises the following raw materials in parts by weight: 0.8-1.5 parts curcumin, 25-35 parts polyethylene glycol 6000, 90-120 parts zinc 2-nitrobenzenesulfonate, 450-550 parts silica aerogel powder, 40-60 parts polyether-modified siloxane, and the balance being ethyl acetate, totaling 1000 parts.

2. The test strip for detecting boric acid and / or borates in cosmetics according to claim 1, characterized in that, A colorimetric card (4) is also attached to the PVC base plate (3).

3. A test strip for detecting boric acid and / or borates in cosmetics, characterized in that, The device includes an activated sample pad (1), a functionalized reaction membrane (2), and a PVC base plate (3) that are sequentially bonded together. The activated sample pad (1) is a glass fiber membrane that has been soaked in a pretreatment reagent. The functionalized reaction membrane (2) is a nitrocellulose membrane that has been coated with a colorimetric reagent. The functionalized reaction membrane (2) includes a bonding area (21) and a colorimetric area (22). The activated sample pad (1) is located in the bonding area (21), and the colorimetric area (22) is exposed to the environment. Based on the total weight of the pretreatment reagent, the pretreatment reagent comprises the following raw materials in parts by weight: 40-60 parts alkyl glycoside, 130-170 parts triethyl orthoformate, 180-250 parts cyclohexanediol dicarboxylate, 90-130 parts camphor sulfonic acid, 45-60 parts polyethylene glycol 400, 25-35 parts bentonite, 15-25 parts cetyltrimethylammonium bromide, and the balance being anhydrous ethanol, totaling 1000 parts; Based on the total weight of the colorimetric reagent, the colorimetric reagent comprises the following raw materials in parts by weight: 0.8-1.5 parts curcumin, 25-35 parts polyethylene glycol 6000, 90-120 parts zinc 2-nitrobenzenesulfonate, 450-550 parts silica aerogel powder, 40-60 parts polyether-modified siloxane, and the balance being ethyl acetate, totaling 1000 parts.

4. A test strip for detecting boric acid and / or borates in cosmetics, characterized in that, The device includes an activated sample pad (1), a functionalized reaction membrane (2), and a PVC base plate (3) that are sequentially bonded together. The activated sample pad (1) is a glass fiber membrane that has been soaked in a pretreatment reagent. The functionalized reaction membrane (2) is a nitrocellulose membrane that has been coated with a colorimetric reagent. The functionalized reaction membrane (2) includes a bonding area (21) and a colorimetric area (22). The activated sample pad (1) is located in the bonding area (21), and the colorimetric area (22) is exposed to the environment. Based on the total weight of the pretreatment reagent, the pretreatment reagent comprises the following raw materials in parts by weight: 40-60 parts alkyl glycoside, 130-170 parts triethyl orthoformate, 180-250 parts cyclohexanediol dicarboxylate, 90-130 parts camphor sulfonic acid, 45-60 parts polyethylene glycol 400, 25-35 parts bentonite, 15-25 parts hexadecyltrimethylammonium bromide, 20 parts silanized silica, and the balance being anhydrous ethanol, totaling 1000 parts; Based on the total weight of the colorimetric reagent, the colorimetric reagent comprises the following raw materials in parts by weight: 0.8-1.5 parts curcumin, 25-35 parts polyethylene glycol 6000, 90-120 parts zinc 2-nitrobenzenesulfonate, 450-550 parts silica aerogel powder, 40-60 parts polyether-modified siloxane, and the balance being ethyl acetate, totaling 1000 parts.

5. A test strip for detecting boric acid and / or borates in cosmetics, characterized in that, The device includes an activated sample pad (1), a functionalized reaction membrane (2), and a PVC base plate (3) that are sequentially bonded together. The activated sample pad (1) is a glass fiber membrane that has been soaked in a pretreatment reagent. The functionalized reaction membrane (2) is a nitrocellulose membrane that has been coated with a colorimetric reagent. The functionalized reaction membrane (2) includes a bonding area (21) and a colorimetric area (22). The activated sample pad (1) is located in the bonding area (21), and the colorimetric area (22) is exposed to the environment. Based on the total weight of the pretreatment reagent, the pretreatment reagent comprises the following raw materials in parts by weight: 40-60 parts alkyl glycoside, 130-170 parts triethyl orthoformate, 180-250 parts cyclohexanediol dicarboxylate, 90-130 parts camphor sulfonic acid, 45-60 parts polyethylene glycol 400, and the balance being anhydrous ethanol, totaling 1000 parts. Based on the total weight of the colorimetric reagent, the colorimetric reagent comprises the following raw materials in parts by weight: 0.8-1.5 parts curcumin, 25-35 parts polyethylene glycol 6000, 90-120 parts zinc 2-nitrobenzenesulfonate, 450-550 parts silica aerogel powder, 40-60 parts polyether-modified siloxane, 30-50 parts ammonium molybdate, with the balance being ethyl acetate, totaling 1000 parts.

6. A test strip for detecting boric acid and / or borates in cosmetics, characterized in that, The device includes an activated sample pad (1), a functionalized reaction membrane (2), and a PVC base plate (3) that are sequentially bonded together. The activated sample pad (1) is a glass fiber membrane that has been soaked in a pretreatment reagent. The functionalized reaction membrane (2) is a nitrocellulose membrane that has been coated with a colorimetric reagent. The functionalized reaction membrane (2) includes a bonding area (21) and a colorimetric area (22). The activated sample pad (1) is located in the bonding area (21), and the colorimetric area (22) is exposed to the environment. Based on the total weight of the pretreatment reagent, the pretreatment reagent comprises the following raw materials in parts by weight: 40-60 parts alkyl glycoside, 130-170 parts triethyl orthoformate, 180-250 parts cyclohexanediol dicarboxylate, 90-130 parts camphor sulfonic acid, 45-60 parts polyethylene glycol 400, 25-35 parts bentonite, 15-25 parts cetyltrimethylammonium bromide, and the balance being anhydrous ethanol, totaling 1000 parts; Based on the total weight of the colorimetric reagent, the colorimetric reagent comprises the following raw materials in parts by weight: 0.8-1.5 parts curcumin, 25-35 parts polyethylene glycol 6000, 90-120 parts zinc 2-nitrobenzenesulfonate, 450-550 parts silica aerogel powder, 40-60 parts polyether-modified siloxane, 30-50 parts ammonium molybdate, with the balance being ethyl acetate, totaling 1000 parts.

7. A test strip for detecting boric acid and / or borates in cosmetics, characterized in that, The device includes an activated sample pad (1), a functionalized reaction membrane (2), and a PVC base plate (3) that are sequentially bonded together. The activated sample pad (1) is a glass fiber membrane that has been soaked in a pretreatment reagent. The functionalized reaction membrane (2) is a nitrocellulose membrane that has been coated with a colorimetric reagent. The functionalized reaction membrane (2) includes a bonding area (21) and a colorimetric area (22). The activated sample pad (1) is located in the bonding area (21), and the colorimetric area (22) is exposed to the environment. Based on the total weight of the pretreatment reagent, the pretreatment reagent comprises the following raw materials in parts by weight: 40-60 parts alkyl glycoside, 130-170 parts triethyl orthoformate, 180-250 parts cyclohexanediol dicarboxylate, 90-130 parts camphor sulfonic acid, 45-60 parts polyethylene glycol 400, 25-35 parts bentonite, 15-25 parts hexadecyltrimethylammonium bromide, 20 parts silanized silica, and the balance being anhydrous ethanol, totaling 1000 parts; Based on the total weight of the colorimetric reagent, the colorimetric reagent comprises the following raw materials in parts by weight: 0.8-1.5 parts curcumin, 25-35 parts polyethylene glycol 6000, 90-120 parts zinc 2-nitrobenzenesulfonate, 450-550 parts silica aerogel powder, 40-60 parts polyether-modified siloxane, 30-50 parts ammonium molybdate, with the balance being ethyl acetate, totaling 1000 parts.

8. A method for detecting boric acid and / or borates in cosmetics, characterized in that, Includes the following steps: S1. The pretreatment reagent includes the following raw materials in parts by weight: 40-60 parts alkyl glycoside, 130-170 parts triethyl orthoformate, 180-250 parts cyclohexanediol dicarboxylate, 90-130 parts camphor sulfonic acid, 45-60 parts polyethylene glycol 400, and the balance being anhydrous ethanol, totaling 1000 parts. According to the proportion, alkyl glycoside, triethyl orthoformate, cyclohexanedimethyl dimethyl ester, camphor sulfonic acid, polyethylene glycol 400 and anhydrous ethanol are mixed evenly to obtain a pretreatment reagent. The glass fiber membrane is immersed in the pretreatment layer solution and then taken out and dried to obtain the activated sample pad (1). S2. The colorimetric reagent comprises the following raw materials in parts by weight: 0.8-1.5 parts curcumin, 25-35 parts polyethylene glycol 6000, 90-120 parts zinc 2-nitrobenzenesulfonate, 450-550 parts silica aerogel powder, 40-60 parts polyether-modified siloxane, and the balance being ethyl acetate, totaling 1000 parts. According to the proportion, curcumin, polyethylene glycol 6000, zinc 2-nitrobenzenesulfonate, silica aerogel powder, polyether modified siloxane and ethyl acetate are mixed evenly to obtain a colorimetric reagent. The colorimetric reagent is coated on the surface of nitrocellulose membrane and cured to obtain a functionalized reaction membrane (2). S3. The functionalized reaction membrane (2) is attached to the PVC base plate (3). The surface of the functionalized reaction membrane (2) is divided into an attachment area (21) and a color development area (22). The activated sample pad (1) is attached to the attachment area (21) of the functionalized reaction membrane (2). The color development area (22) is exposed to the environment to obtain the test strip card. S4. Dissolve the cosmetic to be tested in deionized water, centrifuge, and collect the lower clear liquid. S5. Add the lower clear liquid droplet to the surface of the activated sample pad (1) of the test paper, let it stand for 25-30 seconds, and observe the color change of the functionalized reaction membrane (2) to perform qualitative detection of boric acid and / or borate.

9. The method for detecting boric acid and / or borates in cosmetics according to claim 8, characterized in that, In step S3: the functionalized reaction membrane (2) and the colorimetric card (4) are both attached to the PVC base plate (3). The surface of the functionalized reaction membrane (2) is divided into an attachment area (21) and a color development area (22). The activated sample pad (1) is attached to the attachment area (21) of the functionalized reaction membrane (2). The color development area (22) is exposed to the environment to obtain the test strip card.

10. The method for detecting boric acid and / or borates in cosmetics according to claim 9, characterized in that, In step S5: the lower clear liquid is dropped onto the surface of the activated sample pad (1) of the test paper card, left to stand for 25-30 seconds, and the final color development of the functionalized reaction membrane (2) is observed. The color of the functionalized reaction membrane (2) is compared with the colorimetric card (4). Based on the final color development of the functionalized reaction membrane (2), it is determined whether the cosmetic to be tested contains boric acid and / or borates, and the content of boric acid and / or borates in the cosmetic to be tested is high or low.

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