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GB/T 35948-2018 PDF English

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GB/T 35948-2018: Determination of seven parabens in cosmetics - High performance liquid chromatography
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GB/T 35948-2018: Determination of seven parabens in cosmetics - High performance liquid chromatography


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GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 71.100.70 Y 42 Determination of seven parabens in cosmetics - High performance liquid chromatography Issued on: FEBRUARY 6, 2018 Implemented on: SEPTEMBER 1, 2018 Issued by. General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China; Standardization Administration of the People's Republic of China.

Table of Contents

Foreword ... 3 Introduction ... 4 1 Scope ... 5 2 Normative references ... 5 3 Principle ... 5 4 Reagents and materials ... 6 5 Apparatus ... 6 6 Analytical procedures ... 7 7 Result calculation ... 9 8 Recovery and accuracy ... 9 9 Admissible error ... 9 Annex A (Informative) Chinese names, English names, CAS numbers, molecular formulas, relative molecular masses and constitutional formulas of paraben standard substances ... 10 Annex B (Informative) Liquid chromatograms and spectrograms of seven paraben standard substance solutions ... 11 Determination of seven parabens in cosmetics - High performance liquid chromatography

1 Scope

This Standard specifies the reagents and materials, apparatus, analytical procedures, result calculation, recovery and accuracy, admissible error, etc. for the determination of seven parabens in cosmetics using high performance liquid chromatography, including propylparaben, isopropylparaben, butylparaben, isobutylparaben, phenylparaben, benzylparaben and pentylparaben. This Standard applies to the determination of seven parabens in cosmetics of creams, emulsions, gels, waters, powders, wax base, including propylparaben, isopropylparaben, butylparaben, isobutylparaben, phenylparaben, benzylparaben and pentylparaben. The method detection limits of this Standard. all the method detection limits of seven parabens are 2 mg/kg. The method quantitation limits of this Standard. all the method quantitation limits of seven parabens are 6 mg/kg.

2 Normative references

The following referenced documents are indispensable for the application of this document. For dated references, only the edition dated applies to this document. For undated references, the latest edition of the referenced documents (including all amendments) applies to this document. GB/T 6682, Water for analytical laboratory use – Specification and test methods

3 Principle

Use ethanol 95% to extract sample of cosmetics of creams, emulsions, gels and waters; use acetonitrile to extract sample of powder cosmetics; use cyclohexane to disperse sample wax base cosmetics before using acetonitrile to extract; centrifuge and filter extract before using high performance liquid chromatography for determination. Carry out qualitative analysis based on the retention time and chromatogram and quantitative

6 Analytical procedures

6.1 Sample treatment 6.1.1 Sample of creams, emulsions, gels and waters Weigh 0.5 g (accurate to 0.001 g) of sample to pour into a 10 mL graduated centrifugal tube with a stopper; add 8 mL of ethanol 95% (4.3); vibrate to mix up on vortex mixer (5.3); carry out ultrasonic extraction for 15 min; cool to room temperature; use ethanol 95% to add to metered volume of 10 mL. Take 2 mL of solution to a centrifugal tube; centrifuge for 2 min at 10 000 r/min; carry out determination after filtering using filter membrane (4.8). 6.1.2 Powder sample Weigh 0.5 g (accurate to 0.001 g) of sample to pour into a 10 mL graduated centrifugal tube with a stopper; add 4 mL of acetonitrile (4.2); vibrate on vortex mixer for 1 min; carry out ultrasonic extraction for 15 min; centrifuge for 2 min at 2 000 r/min; transfer all liquid supernatant to a 10 mL colorimetric tube; add 4 mL of acetonitrile (4.2) to residuals to repeat extraction once; combine liquid supernatants; use acetonitrile (4.2) to add to metered volume of 10 mL. Take 2 mL of solution to a centrifugal tube; centrifuge for 2 min at 10 000 r/min; carry out determination after filtering using filter membrane (4.8). 6.1.3 Wax base sample Weigh 0.5 g (accurate to 0.001 g) of sample to pour into a 10 mL graduated centrifugal tube with a stopper; add 2 mL of cyclohexane (4.4); vibrate to mix up on vortex mixer; add 4 mL of acetonitrile (4.2) to vibrate on vortex mixer for 1 min; carry out ultrasonic extraction for 15 min; centrifuge for 2 min at 2 000 r/min; transfer all liquid supernatant to a 10 mL colorimetric tube; add 4 mL of acetonitrile (4.2) to residuals to repeat extraction once; combine liquid supernatants; use acetonitrile (4.2) to add to metered volume of 10 mL. Take 2 mL of solution to a centrifugal tube; centrifuge for 2 min at 10 000 r/min; carry out determination after filtering using filter membrane (4.8). 6.2 Determination 6.2.1 Reference working conditions for high performance liquid chromatography The reference working conditions for high performance liquid chromatography are as follows. a) chromatographic column. core-shell type C18, 2.7 μm, 100 mm × 4.6 mm; or equivalent;

7 Result calculation

The content of parabens in sample is calculated in accordance with the following equation. where. Xi – the content tested constituents in sample, in mg/kg; ci – the mass concentration of tested constituents in sample solution obtained from standard curve, in mg/L; c0 – the mass concentration of tested constituents in blank sample obtained from standard curve, in mL; V – the metered volume of sample solution, in mL; m – the mass of sample, in g; f – the dilution ratio. Result is rounded off to two significant digits.

8 Recovery and accuracy

Within the range of adding concentration of 6 mg/kg ~ 60 mg/kg, the recovery is between 85% ~ 110% and the relative standard deviation is less than 10%.

9 Admissible error

The absolute difference between the results of two tests which are obtained independently under repeatable conditions, shall not exceed 10% of the arithmetic mean value. ......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.


      

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