Method for determining acrylic acid content in carbomer

A technology of acrylic acid and carbomer, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of unsatisfactory sensitivity and separation, cumbersome operation, and affecting measurement results, so as to prevent potential harm to health and sensitivity With the effect of high precision and overcoming cumbersome operation

Inactive Publication Date: 2017-05-24
贵州省欣紫鸿药用辅料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the detection method of acrylic acid in carbomer is mostly potentiometric titration, but this method is cumbersome to operate and has low sensitivity; with the continuous development of science, the research of gas chromatography and high performance liquid chromatography is on the rise. Generally speaking, high performance liquid chromatography is suitable for the determination of difficult volatile substances, and gas chromatography is suitable for the detection of volatile substances, but the sensitivity and resolution are still not ideal, and the system error is still relatively large; in addition, direct gas chromatography or High-performance liquid chromatography is used to detect carbomer samples, which may easily cause problems such as high polymer contamination of the chromatograph, which will further affect the measurement results

Method used

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  • Method for determining acrylic acid content in carbomer
  • Method for determining acrylic acid content in carbomer
  • Method for determining acrylic acid content in carbomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] S1. Preparation of working standard solution:

[0031] Take acrylic acid (analytical pure), put it in a 10mL stoppered colorimetric tube, dilute to the mark with methanol, mix well, put it in a 10mL stoppered centrifuge tube, centrifuge at 5000r / min for 3min, take the supernatant with 0.22 The μm organic filter membrane is filtered, and the filtrate is used as a standard solution, and the concentration of the working standard solution is shown in Table 1:

[0032] Table 1:

[0033] Standard solution series 1# 2# 3# 4# 5# 6# Acrylic acid (μg / mL) 10 2 1 0.4 0.2 0.1

[0034] S2, sample processing:

[0035] Weigh 1.0g sample, place it in a microwave extraction tube, add 15mL N,N-dimethylformamide, place the microwave extraction tube in a microwave extraction apparatus, extract at 130°C for 20min, centrifuge, and take the The clear liquid was filtered with a 0.22 μm organic filter membrane, and the filtrate was obtained as the sample solution...

Embodiment 2

[0061] The difference from Example 1 is that on the basis of "sample treatment" and "detection method", the working standard solution series and sample solution of acrylic acid are determined;

[0062] The differences are as follows:

[0063] Sample treatment: Weigh 1.0g sample, place it in a microwave extraction tube, add 15mL tetrahydrofuran, place the microwave extraction tube in a microwave extraction apparatus, extract at 120°C for 20min, centrifuge, take the supernatant and wash it with 0.22μm Filter with an organic membrane to obtain the filtrate as the sample solution;

[0064] Detection method: chromatographic column: SFC capillary column; stationary phase: silica gel; column temperature: 36°C; injection volume: 20μL; mobile phase: N2O; detection wavelength: 290nm; constant pressure: 71.7×10 6Pa; Split ratio: 10:1; Detection point: FID, 250°C; Gas supply: nitrogen;

[0065] The test results are as follows:

[0066] Linear regression equation: y=83.57x+1.43, the cor...

Embodiment 3

[0077] On the basis of the difference from Example 1 in "sample treatment" and "detection method", the working standard solution series and sample solution of acrylic acid are measured;

[0078] The differences are as follows:

[0079] Sample treatment: Weigh 1.0g sample, place it in a microwave extraction tube, add 15mL cyclohexane, place the microwave extraction tube in a microwave extraction apparatus, extract at 140°C for 15min, centrifuge, and take the supernatant for use Filter through a 0.22 μm organic filter membrane to obtain the filtrate as the sample solution;

[0080] Detection method: chromatographic column: SFC capillary column; stationary phase: silica gel; column temperature: 38°C; injection volume: 30μL; mobile phase: N2O; detection wavelength: 320nm; constant pressure: 71.7×10 6 Pa; Split ratio: 10:1; Detection point: FID, 250°C; Gas supply: nitrogen;

[0081] The test results are as follows:

[0082] Linear regression equation: y=85.12x-0.98, the correlat...

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Abstract

The invention relates to an acrylic acid detection technique, and particularly relates to a method for determining the acrylic acid content in carbomer. The method comprises the steps of firstly, mixing a to-be-determined product with an extraction agent according to the massic volume ratio of 1:(12 to 18), performing microwave extraction for 15 to 20 min at 120 to 140 DEG C, centrifugalizing, then filtering supernate so as to obtain filtrate, and then quantitatively determining the acrylic acid content in the carbomer with supercritical fluid chromatography and an external standard method, wherein chromatographic conditions include that a chromatographic column is an SFC capillary column, the stationary phase is silica gel, the column temperature is 36 to 38 DEG C, the injection volume is 20 to 30 muL, the moving phase is N2O, the detection wavelength is 290 to 320 nm, the constant pressure is 71.7*10<6> Pa, the split ratio is 10:1, a detection point is an FID (Flame Ionization Ditector) at 250 DEG C, and the supplementary gas is nitrogen. The method which is used for determining acrylic acid in the carbomer has the advantages of simplicity and convenience in operation and high sensitivity and precision.

Description

technical field [0001] The invention relates to acrylic acid detection technology, in particular to a method for measuring acrylic acid content in carbomer. Background technique [0002] Carbomer, also known as Carbopol, chemical name: cross-linked polyacrylic acid resin, is a high molecular polymer cross-linked by acrylic acid and propylene-based sucrose or propylene-based pentaerythritol. Carbomer has good gelation properties , viscosity, thickening, emulsifying, suspending and film-forming properties, and the chemical properties are stable and safe, without irritation and allergic reactions, and it has good compressibility under low pressure, and it is compatible with most other excipients With good compatibility, it is widely used in daily chemicals, textiles, coatings, food, construction, medical treatment, electronics and other fields. [0003] Acrylic acid is an organic compound with a strong pungent odor. It is a colorless liquid at room temperature and can irritate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 沈惠洪怡母逸青
Owner 贵州省欣紫鸿药用辅料有限公司
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