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Textiles - Determination of benzalkonium chloride
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GB/T 43721-2024: Textiles - Determination of benzalkonium chloride---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT43721-2024
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 59.080.01
CCS W 04
GB/T 43721-2024
Textiles - Determination of benzalkonium chloride
Issued on: MARCH 15, 2024
Implemented on: OCTOBER 01, 2024
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 Terms and definitions... 4
4 Principle... 4
5 Reagents and materials... 4
6 Instruments... 5
7 Test steps... 6
8 Calculation and expression of results... 8
9 Detection limit, limit of quantification and precision... 9
10 Test report... 9
Annex A (normative) Chemical information of benzalkonium chloride... 11
Annex B (informative) HPLC-DAD analysis conditions... 12
Annex C (informative) High performance liquid chromatogram and spectrum of
benzalkonium chloride... 13
Annex D (informative) HPLC-MS/MS analysis conditions... 16
Annex E (informative) Multiple reaction monitoring selected ion flow chromatogram
of benzalkonium chloride... 18
Textiles - Determination of benzalkonium chloride
WARNING -- Persons using this document shall be familiar with normal
laboratory practice. This document does not purport to address all of the safety
problems, if any, associated with its use. It is the responsibility of the user to
establish appropriate safety and health practices and to ensure compliance with
any national regulatory conditions.
1 Scope
This document describes the test methods for the determination of benzalkonium
chloride in textiles using high performance liquid chromatography-diode array detector
(HPLC-DAD) or high performance liquid chromatography-tandem mass spectrometry
(HPLC-MS/MS).
This document applies to all types of textile products.
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 Water for analytical laboratory use - Specification and test methods
3 Terms and definitions
For the purpose of this document, there are no terms and definitions that need to be
defined.
4 Principle
Use acetonitrile to ultrasonically extract the benzalkonium chloride in the sample, after
the extract is filtered through a filter membrane, it is determined by HPLC-DAD or
HPLC-MS/MS and quantified by the external standard method.
5 Reagents and materials
Unless otherwise specified, all reagents are at least analytical grade.
5.1 Water. grade 2 water as specified in GB/T 6682.
5.2 Acetonitrile. CAS No. 75-05-8, chromatographic grade.
5.3 Methanol. CAS No. 67-56-1, chromatographic grade.
5.4 Formic acid. CAS No. 64-18-6.
5.5 Ammonium acetate. CAS No. 631-61-8.
5.6 Glacial acetic acid. CAS No. 64-19-7.
5.7 Three kinds of benzalkonium chloride standard substances. comply with the
provisions of Annex A, purity ≥ 97.0 %.
5.8 Mixed standard stock solution. Use an analytical balance (6.3) to weigh a certain
amount of each benzalkonium chloride standard substance (5.7), dissolve and make up
to the mark with acetonitrile (5.2), to prepare a mixed standard stock solution with a
mass concentration of 1000 mg/L.
NOTE. The mixed standard stock solution is stored in a refrigerator at 0 ℃ ~ 8 ℃ and has a shelf
life of 6 months.
5.9 Mixed standard working solution. Accurately pipette a certain volume of the mixed
standard stock solution (5.8) and dilute with acetonitrile (5.2) to obtain series mixed
standard working solutions of at least 5 different concentrations. When using HPLC-
DAD for analysis, prepare mixed standard working solutions of a series of
concentrations, such as 5.0 mg/L, 10.0 mg/L, 20.0 mg/L, 50.0 mg/L, and 100.0 mg/L;
when using HPLC-MS/MS for analysis, prepare mixed standard working solutions of
a series of concentrations, such as 0.05 mg/L, 0.10 mg/L, 0.20 mg/L, 0.50 mg/L, and
1.00 mg/L. This solution is prepared and used immediately.
5.10 Ammonium acetate solution. Weigh 7.70 g of ammonium acetate (5.5) and place
in a beaker, add water (5.1) to dissolve and dilute to 1000 mL, adjust the pH to 5.0 with
glacial acetic acid (5.6), and filter with an aqueous filter membrane (5.13).
5.11 0.1 % formic acid solution. Pipette 1 mL of formic acid (5.4) into a 1000 mL
volumetric flask and make up to the mark with water (5.1).
5.12 Organic phase filter membrane. pore size 0.22 μm, made of
polytetrafluoroethylene (PTFE).
5.13 Aqueous phase filter membrane. pore size 0.22 μm, made of mixed cellulose ester
(MCE).
6 Instruments
6.1 High performance liquid chromatograph (HPLC). equipped with a diode array
detector (DAD).
6.2 High performance liquid chromatography-tandem mass spectrometer (HPLC-
MS/MS). equipped with an electrospray ionization source (ESI).
6.3 Analytical balance. the graduation values are 0.01 g and 0.0001 g.
6.4 Ultrasonic water bath generator. the working frequency is (40 ± 5) kHz, the water
bath temperature can be controlled at (60 ± 3) ℃.
6.5 pH meter. the graduation value is 0.01.
6.6 Glass container. 40 mL ~ 60 mL, made of hard glass, with a screw-on sealing cover.
6.7 Volumetric flask. 1000 mL.
7 Test steps
7.1 Sample preparation
Take a representative sample, cut it into pieces less than 5 mm × 5 mm, and mix it
thoroughly.
7.2 Sample extraction
Weigh (1 ± 0.1) g of sample, accurate to 0.01 g, place in a glass container (6.6), add 20
mL of acetonitrile (5.2), tighten the sealing cover, place in a (60 ± 3) ℃ ultrasonic water
bath generator (6.4) for ultrasonic extraction for (30 ± 1) min, take out the glass
container (6.6) and cool to room temperature, take part of the extract and filter through
the organic phase filter membrane (5.12), and the filtrate is used as the test liquid for
analysis on the instrument.
7.3 HPLC-DAD analysis
Under the same test conditions, take equal volumes of the test solution obtained in 7.2
and the mixed standard working solution (5.9) and alternately inject them for
determination. The HPLC-DAD analysis conditions are shown in Annex B. Qualitative
analysis is performed by comparing the retention time of the chromatographic peak at
a specific detection wavelength and the ultraviolet absorption spectrum. If the relative
deviation between the retention time of the target analyte in the test solution and the
retention time corresponding to the standard substance is within the range of ±2.5 %,
the ultraviolet absorption spectrum is consistent with that of the standard substance, and
the maximum absorption wavelength deviation is within the range of ±2 nm, it can be
determined that the corresponding target analyte exists in the sample.
Under the HPLC-DAD analysis conditions given in Annex B, the chromatogram and
spectrum of benzalkonium chloride obtained are shown in Annex C.
According to the content of the target analyte in the test solution, select a mixed
standard working solution (5.9) with a similar response value for analysis. With the
response peak area of the target analyte as the vertical axis and the concentration of the
target analyte as the horizontal axis, plot a standard working curve, and perform
quantitative analysis according to the external standard method. The response values of
the target analyte in the mixed standard working solution (5.9) and the test solution
obtained in 7.2 shall be within the linear response range of the instrument. If the content
exceeds the range of the standard curve, dilute with acetonitrile to an appropriate
concentration before determination.
7.4 HPLC-MS/MS analysis
Under the same test conditions, take equal volumes of the test solution obtained in 7.2
and the mixed standard working solution (5.9) and alternately inject them for
determination. The HPLC-MS/MS analysis conditions are shown in Annex D. Compare
the retention times of the mass chromatographic peaks of the test solution and the mixed
standard working solution (5.9). If the relative deviation between the retention time of
the target analyte in the test solution and the retention time corresponding to the
standard substance is within the range of ±2.5 %, and the deviation between the relative
ion abundance of the qualitative ion pair and the relative ion abundance of the standard
working solution with equivalent concentration do not exceed the range specified in
Table 1, it can be determined that the corresponding target analyte exists in the sample.
Under the HPLC-MS/MS analysis conditions given in Annex D, the multiple reaction
monitoring selected ion current chromatogram of each benzalkonium chloride is shown
in Annex E.
According to the content of the target analyte in the test solution, select a mixed
standard working solution (5.9) with a similar response value for analysis. Use the
response peak area of the target analyte as the vertical axis and the concentration of the
target analyte as the horizontal axis, plot a standard working curve, and perform
quantitative calculation according to the external standard method. The response values
of the target analyte in the mixed standard working solution (5.9) and the test solution
obtained in 7.2 shall be within the linear response range of the instrument. If the content
exceeds the range of the standard curve, dilute with acetonitrile to an appropriate
concentration before determination.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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