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GB/T 41412-2022 English PDF (GBT41412-2022)

GB/T 41412-2022 English PDF (GBT41412-2022)

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GB/T 41412-2022: Determination of isothiazolinone preservatives in toys -- High performance liquid chromatography-tandem mass spectrometry
GB/T 41412-2022
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 97.200.50
CCS Y 57
Determination of isothiazolinone preservatives in toys - High
performance liquid chromatography-tandem mass
spectrometry
ISSUED ON: APRIL 15, 2022
IMPLEMENTED ON: APRIL 15, 2022
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 ... 5 
6 Instruments and equipment ... 5 
7 Pre-preparation of sample ... 6 
8 Determination ... 6 
9 Result calculation ... 8 
10 Method limits of quantification ... 9 
11 Precision ... 9 
12 Test report ... 9 
Annex A (normative) Information on the target substances (3 preservatives) determined
in this document ... 10 
Annex B (informative) Total ion chromatogram of 3 preservatives ... 11 
Annex C (informative) Precision test results ... 12 
Determination of isothiazolinone preservatives in toys - High
performance liquid chromatography-tandem mass
spectrometry
WARNING -- Persons using this document should have practical experience with
formal laboratory work. This document does not address all possible security
issues. It is the user's responsibility to take appropriate safety and health measures,
and to ensure compliance with the conditions stipulated by relevant national
regulations.
1 Scope
This Standard specifies high performance liquid chromatography-tandem mass
spectrometry for determination of isothiazolinone preservatives in toys.
This Standard applies to determination of 2-methyl-4-isothiazolin-3-one (MIT), 5-
chloro-2-methyl-4-isothiazolin-3-one (CMIT) and 1,2-benzisothiazoline- 3-ketone
(BIT) in toys. Other preservatives can be determined with reference to this document
after verification.
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
There are no terms and definitions that need to be defined in this document.
4 Principle
After the sample is prepared, use methanol to conduct ultrasonic extraction at room
temperature. The extract is filtered by a filter membrane and then determined by high
performance liquid chromatography-tandem mass spectrometer. Quantify by internal
standard method.
5 Reagents and materials
5.1 Water: Grade 1 water specified in GB/T 6682.
5.2 Methanol: Chromatographically pure.
5.3 Preservative standard material: Purity is ≥95%; Annex A gives the specific
information of MIT, CMIT and BIT.
5.4 Internal standard substance: 2-methyl-4-isothiazolin-3-one-d3 hydrochloride salt,
referred to as MIT-d3, CAS No. is 1329509-49- 0; Purity is ≥95%.
5.5 Internal standard substance: 5-chloro-2-methyl-4-isothiazolin-3-one-d3, referred to
as CMIT-d3, CAS No. is 1329611-34-8); Purity is ≥95%.
5.6 Internal standard substance: 1,2-benzisothiazolin-3-one-13C6, referred to as BIT-
13C6, CAS No. is 1329616-16-1; Purity is ≥95%.
5.7 Standard stock solution: Respectively and accurately weigh an appropriate amount
of preservative reference material (5.3). Use methanol (5.2) to prepare a standard stock
solution with a mass concentration of 100.0mg/L.
5.8 Internal standard mixed solution: Accurately weigh an appropriate amount of
internal standard substances MIT-d3 (5.4), CMIT-d3 (5.5) and BIT-13C6 (5.6). Use
methanol (5.2) to dilute and obtain internal standard mixed solutions with mass
concentrations of 1.0mg/L, 3.0mg/L and 1.0mg/L, respectively.
5.9 Standard mixed working solution: Pipette an appropriate volume of the preservative
standard stock solution (5.7) into a volumetric flask. Use methanol (5.2) to set volume
to the scale mark. Obtain a standard mixed solution with a mass concentration of
10.0mg/L. Use methanol (5.2) and stepwise dilution method to dilute the standard
mixed solution and obtain a series of standard mixed working solutions with mass
concentrations of 0.0005mg/L, 0.001mg/L, 0.005mg/L, 0.01mg/L, 0.02mg/L and
0.05mg/L. Take 1.0mL of a series of standard mixed working solutions into the injection
bottle. Add 0.050mL of internal standard mixed solution (5.8). Mix well.
5.10 Microporous membrane: Organic phase, with a pore size of 0.22μm.
6 Instruments and equipment
6.1 High performance liquid chromatography-tandem mass spectrometer: Equipped
with electrospray ionization (ESI).
6.2 Ultrasonic extractor.
6.3 Analytical balance: Accuracy is 0.1 mg.
Keep 3 significant digits.
10 Method limits of quantification
The method limits of quantification for MIT, CMIT and BIT in this document are all
0.040mg/kg.
11 Precision
See Annex C for the precision test results of the method in this document.
12 Test report
The test report shall at least give the following information:
a) Specimen description;
b) Reference (including the year number) to this document;
c) Test results;
d) Variations from the prescribed analysis steps;
e) Anomalies observed in tests;
f) Test date.

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