GB/T 38741-2020Oral care and cleansing products—Determination of chlorhexidine, furacin, diclofenac, chloroxylenol and hexamidine diisethionate in toothpastes—High performance liquid chromatography (English PDF)

Foreword

This standard was drafted in accordance with the rules given in GB/T 1.1-2009.

1 Scope

This standard stipulates five kinds of sterilization of chlorhexidine, furancillin, diclofenac, chloroxylenol and hexamidine bis (hydroxyethylsulfonate) salt in toothpaste Principles, reagents or materials, instruments and equipment, test procedures, test data processing, detection limits and quantification of the determination of reagent content by high performance liquid chromatography Limits, recovery and precision.

This standard is applicable to the content of chlorhexidine, furancillin, diclofenac, chloroxylenol, and hexamidine bis (hydroxyethylsulfonate) in toothpaste. Determination.

2 Normative references

The following documents are essential for the application of this document. For dated references, only the dated version applies to this document. For the cited documents without date, the latest version (including all amendments) applies to this document.

GB/T 6682 Analysis laboratory water specifications and test methods

3 Principle

After ultrasonic extraction of the formic acid-methanol-water mixed solution, the sample was determined by high-performance liquid chromatography, qualitative by retention time, and quantified by external standard method.

4 Reagents or materials

Unless otherwise stated, the reagents used are of analytical grade, and the water is the first grade water specified in GB/T 6682.

4.1 Formic acid. chromatographically pure.

4.2 Trifluoroacetic acid. chromatographically pure.

4.3 Methanol. chromatographic grade.

4.4 0.1% formic acid in methanol. Pipette 1mL of formic acid (see 4.1) accurately and dilute to 1L with methanol (see 4.3).

4.5 0.1% formic acid solution. Pipette 1mL formic acid accurately (see 4.1), dilute to 1L with water.

4.6 Formic acid-methanol-water mixed solution. accurately measure 80mL of 0.1% formic acid in methanol (see 4.4) and 20mL of 0.1% formic acid in solution (see 4.5), mix well.

4.7 0.1% trifluoroacetic acid methanol solution. accurately transfer 1mL trifluoroacetic acid (see 4.2), diluted with methanol (see 4.3) to 1L.

4.8 0.1% trifluoroacetic acid solution. Pipette 1mL trifluoroacetic acid accurately (see 4.2), dilute to 1L with water.

4.9 Reference materials. chlorhexidine, furancillin, diclofenac, chloroxylenol, and hexamidine di (hydroxyethylsulfonate) salt, purity >=98% For the article name, English name, CAS number, molecular formula, relative molecular mass and structural formula, see Table A.1 in Appendix A.

4.10 Standard stock solution (each 1000mg/L). accurately weigh the standard substance of hexamidine bis (hydroxyethylsulfonate) salt (see 4.9) 0.1g (accurate To 0.1mg), placed in a 100mL brown volumetric flask, dissolved in water and made to volume. Accurately weigh chlorhexidine, furacillin, diclofenac, chlorodi