ISO 22992-2:2020 pdf download

ISO 22992-2:2020 pdf download.Textiles — Determination of certain preservatives — Part 2: Determination of triclosan residues method using LC-MS/ MS
1 Scope
This document specifies a method for determination of triclosan residues in textiles by high performance liquid chromatography — tandem mass spectrometry (HPLC-MS/MS).
This method is applicable to all kinds of textile products.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content constitutes requirements 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.
ISO 3696, Water for analytical laboratory use — Specification and test methods
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at http:// www .electropedia .org/
4 Principle
The triclosan is extracted from textile specimen by ultrasonic generator with methanol. After being concentrated and diluted to volume, the residue is determined by HPLC-MS/MS, quantified by external standard method.
Statistical data of interlaboratory trial is given in Annex B.
5 Reagents
5.1 Water, grade 1 water specified in ISO 3696.
5.2 Methanol, HPLC grade.
5.3 Triclosan, CAS No. 3380-34-5, with a purity of more than 98 %.
6 Apparatus and materials
6.1 High performance liquid chromatography — tandem mass spectrometry (HPLC-MS/MS),equipped with electrospray ionization source.
6.2 Rotary vacuum evaporator.
6.3 Ultrasonic bath, with controllable heating capable of maintaining a temperature of about 40 °C.
6.4 Nitrogen blowing device.
6.5 Balance, with a resolution of 0,01 g used for preparing test specimen.
6.6 Balance, with a resolution of 0,1 mg used for preparing standard solution.
6.7 Glass vial, with a capacity of 40 ml with tight closure.
7 Test procedure
7.1 Preparation of standard solution
7.1.1 Standard stock solution
Prepare 1 000 mg/l stock standard solution of the triclosan (5.3) in methanol (5.2).
7.1.2 Working solution
Prepare a working solution of the triclosan in methanol and dilute it to a series of suitable concentrations depending on test needs. Select at least five appropriate dilutions of the calibration sets to create calibration curve.
NOTE Standard stock solution is kept in the refrigerator at 0 °C to 4 °C for up to 6 months. Working solution is kept in the refrigerator at 0 °C to 4 °C for up to 3 months.
7.3 Ultrasonic wave extraction
Put the pieces into a vial with tight closure (6.7) and add 25 ml of methanol (5.2). Place the vial in an ultrasonic generator (6.3) at about 40 °C for (30 ± 2) min. Filter and transfer the extract into 100 ml flask (6.8). Add 25 ml of methanol to the residue and place the vial in the ultrasonic generator to extract the residue at about 40 °C for (30 ± 2) min. Filter and merge the extract into the flask (6.8).