GB/T 40190-2021Determination of forbidden bleach in toothpaste—High performance liquid chromatography method (English PDF)
牙膏中禁用漂白剂的测定 高效液相色谱法
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Issued by
SAMR; SAC
Level / Type
National · Recommended
Issue date
May 21, 2021
Implementation date
December 1, 2021
Scope
GB/T 40190-2021 is the English-translated version of 牙膏中禁用漂白剂的测定 高效液相色谱法.
GB/T 40190-2021 is the Chinese national method for detecting benzoyl peroxide, a bleach that is forbidden in toothpaste, by high performance liquid chromatography.
The sample is extracted with acetonitrile and water (80:20 by volume), the supernatant is filtered through a 0.45 µm membrane, and benzoyl peroxide is determined by post-column derivatization with hemin and p-hydroxyphenylacetic acid followed by fluorescence detection, with quantification by external standard peak area.
The standard lists the reagents and instruments, specimen preparation, the chromatographic and derivatization conditions, a five-point calibration series from 10 mg/L to 100 mg/L, the determination steps and blank test, the calculation of results and precision.
Its detection limit is 0.5 mg/kg. It was issued on 21 May 2021 and has applied since 1 December 2021.
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Document preview — GB/T 40190-2021
National Standard of the People's Republic of China
- ICS
- 71.040.40
- Classification
- Y 43
Issued by: State Administration for Market Regulation; Standardization Administration of the PRC
Contents
- Foreword3
- 1 Scope4
- 2 Normative references4
- 3 Principle4
- 4 Reagents and standard materials4
- 5 Instruments5
- 6 Specimen preparation5
- 7 Determination by high performance liquid chromatography5
- 8 Result calculation7
- 9 Precision7
- Annex A (informative) Liquid chromatogram of benzoyl peroxide standard sample8
1 Scope
This Standard specifies high performance liquid chromatography method to determine the content of forbidden bleach - benzoyl peroxide - in toothpaste.
This Standard is applicable to the determination of the content of forbidden bleach - benzoyl peroxide - in toothpaste. The method detection limit of this Standard is 0.5mg/kg.
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.
GB/T 6682-2008, Water for analytical laboratory use - Specification and test methods
3 Principle
Acetonitrile for samples: After water extraction (80:20, volume ratio), after the supernatant is filtered through a 0.45µm filter membrane, use post-column derivatization-high performance liquid chromatography-fluorescence detection method to determine. Use external standard peak area method to quantify.
4 Reagents and standard materials
Unless otherwise specified, all reagents used are analytically-pure AND water is grade one water specified in GB/T 6682-2008.
4.1 Acetonitrile: chromatographically pure.
4.2 Hemin: mass fraction >=98.0%.
4.3 P-hydroxyphenylacetic acid: mass fraction >=98.0%. […]
7 Determination by high performance liquid chromatography
b) Fluorescence detector wavelength: excitation wavelength is 315nm, emission wavelength is 400nm.
c) Mobile phase: methanol with 0.1% acetic acid: water (85:15, volume ratio).
d) Flow rate: 0.6mL/min.
e) Column temperature: 20°C.
f) Injection volume: 10µL.
g) Derivative conditions: The derivatization reagent are 8µmol/L hemin and 80µmol/L p-hydroxyphenylacetic acid in NH4Cl-NH3·H2O buffer solution (pH=10.5). The back pressure of the post-column derivative is 500psi~1000psi or the flow rate is 0.2mL/min. The temperature of the reaction tube is 35°C.
7.2 Preparation of standard working solution
Accurately pipette 1.0mL, 2.0mL, 4.0mL, 8.0mL, 10.0mL of standard stock solution (4.6) in a 100mL volumetric flask. Use acetonitrile to dilute to the scale mark. Shake well. Filter it by 0.45µm filter membrane for future use. At this time, the mass concentration of the standard series solution is 10.0 mg/L, 20.0 mg/L, 40.0 mg/L, 80.0 mg/L, 100.0 mg/L. Under the set chromatographic conditions (7.1), respectively take 10µL for analysis. Take the mass concentration of the standard series solution as the abscissa (mg/L), the peak area of the reference substance as the ordinate to draw the calibration curve (linear correlation coefficient R>=0.9990). Refer to Figure A.1 in Annex A for the liquid chromatogram of benzoyl peroxide standard sample.
7.3 Determination steps
After the sample is processed according to the steps in Chapter 6, perform on-board testing according to the instrument conditions of 7.1. The response value of benzoyl peroxide in the test sample solution shall be within the linear range of the standard curve. If it exceeds the linear range, it shall be diluted before injection for determination.
7.4 Blank test
Except not adding specimen, all are tested in accordance with the processing steps in Chapter 6 and the instrument conditions in 7.1. […]
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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 15 pages — is available in the English PDF.
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