GB/T 40185-2021 PDF in English
GB/T 40185-2021 (GB/T40185-2021, GBT 40185-2021, GBT40185-2021)
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| GB/T 40185-2021 | English | 155 |
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Determination of 5 kinds of ammonium chloride antibacterial agents in toothpaste - High performance liquid chromatography method
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Standards related to (historical): GB/T 40185-2021
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GB/T 40185-2021: PDF in English (GBT 40185-2021) GB/T 40185-2021
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.040.40
Y 43
Determination of 5 kinds of ammonium chloride
antibacterial agents in toothpaste - High performance
liquid chromatography method
ISSUED ON: MAY 21, 2021
IMPLEMENTED ON: DECEMBER 01, 2021
Issued by: State Administration for Market Regulation;
Standardization Administration of the People's Republic of
China.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Principle ... 4
4 Reagents and standard materials ... 4
5 Instruments ... 5
6 Analysis steps ... 5
7 Expression of analysis results ... 7
8 Precision ... 7
9 Recovery rate ... 7
Annex A (informative) Liquid chromatograms of laura ammonium chloride,
benzethonium chloride, cetylpyridinium chloride, mitanium chloride and
sitacium chloride standard material ... 8
Determination of 5 kinds of ammonium chloride
antibacterial agents in toothpaste - High performance
liquid chromatography method
1 Scope
This Standard specifies high performance liquid chromatography (HPLC)
method for the content of ammonium chloride antibacterial agents - laura
ammonium chloride, benzethonium chloride, cetylpyridinium chloride, mitanium
chloride and sitacium chloride - in toothpaste.
This Standard is applicable to the determination of the content of 5 kinds of
ammonium chloride antibacterial agents in toothpaste.
The method detection limit of this Standard is: 0.075g/kg (laura ammonium
chloride, benzethonium chloride), 0.0125g/kg (cetylpyridinium chloride,
methachloride) and 0.025g/kg (sitacium chloride).
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
The sample is ultrasonically extracted and filtered by water and ethanol. Use
high performance liquid chromatography to separate. Use UV to determine.
Use external standard method to quantify.
4 Reagents and standard materials
Unless otherwise specified, it shall only use the confirmed analytically-pure
reagents AND water specified as grade one water in GB/T 6682-2008.
6.3 Determination
6.3.1 Reference conditions of liquid chromatography
The reference conditions of liquid chromatography are as follows:
a) Chromatographic column: CN column (150×4.6mm, 5μm).
b) Mobile phase: Acetonitrile (A) + 0.1% HClO4 aqueous solution (add 1mL
of HClO4 into 1L of water) (B). Use isocratic elution: A/B=40:60 (volume
ratio).
c) Flow rate: 1.0mL/min.
d) Injection volume: 10μL.
e) Column temperature: 30°C.
f) Detection wavelength: 215nm (laura ammonium chloride, mitanium
chloride and sitacium chloride), 225nm (benzethonium chloride), 260nm
(cetylpyridinium chloride).
6.3.2 Drawing of standard working curve
Determine according to liquid chromatography conditions (6.3.1). The linear
range of laura ammonium chloride and benzethonium chloride is 0.001
mg/mL~0.2 mg/mL. The linear range of cetylpyridinium chloride and mitanium
chloride is 0.0015mg/mL~0.2mg/mL. The linear range of sitacium chloride is
0.003mg/mL~0.2mg/mL. For the liquid chromatograms of 5 mixed standard
materials, refer to Figure A.1 ~ Figure A.3 in Annex A.
6.3.3 Quantitative analysis
Determine the test sample solution according to the liquid chromatographic
conditions (6.3.1). Quantify by comparing the peak area with the standard
series. If the response value of the specimen solution exceeds the response
value of the standard series, it is necessary to dilute the specimen by an
appropriate multiple before injection.
6.3.4 Qualitative confirmation
Based on the retention time of the tested component in the standard solution,
perform preliminary characterization. During the determination, if the specimen
solution has a positive result, it shall be compared with the UV absorption
spectrum of the standard product, for qualitative confirmation.
6.4 Blank test
Except for not weighing samples, all follow the above steps.
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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