GB/T 40191-2021Determination of restricted preservatives in toothpaste—High performance liquid chromatography method (English PDF)
牙膏中限用防腐剂的测定 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 40191-2021 is the English-translated version of 牙膏中限用防腐剂的测定 高效液相色谱法.
GB/T 40191-2021 is a high performance liquid chromatography method for measuring two restricted preservatives in toothpaste, sorbic acid and benzoic acid.
The sample is extracted with pure water, centrifuged and filtered through a 0.45 µm membrane, and the extract is separated on a C18 column with a methanol and ammonium acetate mobile phase and detected by ultraviolet absorption at 230 nm.
The two acids are identified by retention time and quantified by external standard peak area against a calibration curve drawn from 5 mg/L to 50 mg/L working solutions.
The method detection limit is 0.5 mg/kg, and the standard also covers reagents, instruments, result calculation and precision, with a chromatogram of the mixed standard in Annex A. It was issued on 21 May 2021 and has applied since 1 December 2021.
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Document preview — GB/T 40191-2021
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 chromatography6
- 8 Result calculation7
- 9 Precision7
- Annex A (informative) Liquid chromatogram of mixed benzoic acid and sorbic acid standard sample8
1 Scope
This Standard specifies high performance liquid chromatography (HPLC) method to determine the content of restricted preservatives - sorbic acid and benzoic acid - in toothpaste.
This Standard is applicable to the determination of the content of restricted preservatives - sorbic acid and benzoic acid - 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
Use pure water to extract the sample. The supernatant is filtered through a 0.45µm filter membrane. Use high performance liquid chromatography-ultraviolet detection method to determine. Use retention time to characterize. 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 Methanol: chromatographically pure. […]
6 Specimen preparation
After shaking for 15min, add pure water to set volume to 25mL. Shake well. Let it still. Transfer the supernatant to the centrifuge tube. Centrifuge at 4000r/min for 10min. Take the supernatant and pass it through the 0.45µm microporous membrane. Inject a sample to test.
7 Determination by high performance liquid chromatography
7.1 Reference conditions of liquid chromatography
The reference conditions of liquid chromatography are as follows:
a) Chromatographic column: C18 stainless steel column (250mm×4.6mm×5µm).
b) Detection wavelength: 230nm.
c) Mobile phase: methanol/ammonium acetate aqueous solution (0.02mol/L) (5:95, volume ratio).
d) Flow rate: 1.0mL/min.
e) Column temperature: 30°C.
f) Injection volume: 10µL.
7.2 Preparation of standard working solution
Use mobile phase solution to gradually dilute the 100mg/L mixed standard solution (4.7). Prepare into 50mg/L, 20mg/L, 10mg/L, 5mg/L standard working solutions. Filter by 0.45µm filter membrane for future use. Under the set chromatographic conditions, respectively take 10µL for analysis. Take the mass concentration of the standard series of solutions 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 the mixed benzoic acid and sorbic acid 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 values of benzoic acid and sorbic acid 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. […]
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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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