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BS ISO 22104:2021

BS ISO 22104:2021

$167.15

Water quality. Determination of microcystins. Method using liquid chromatography and tandem mass spectrometry (LC-MS/MS)

Published By Publication Date Number of Pages
BSI 2021 42
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This document specifies a method for the quantification of twelve microcystin variants (microcystin-LR, -LA, -YR, -RR, -LY, -WR, -HtyR, -HilR, -LW, -LF, [Dha7]-microcystin-LR, and [Dha7]-microcystin-RR) in drinking water and freshwater samples between 0,05 µg/l to 1,6 µg/l. The method can be used to determine further microcystins, provided that analytical conditions for chromatography and mass spectrometric detection has been tested and validated for each microcystin. Samples are analysed by LC-MS/MS using internal standard calibration.

This method is performance based. The laboratory is permitted to modify the method, e.g. increasing direct flow injection volume for low interference samples or diluting the samples to increase the upper working range limit, provided that all performance criteria in this method are met.

Detection of microcystins by high resolution mass spectrometry (HRMS) as an alternative for tandem mass spectrometry (MS/MS) is described in Annex A.

An alternative automated sample preparation method based on on-line solid phase extraction coupled to liquid chromatography is described in Annex B.

When instrumental sensitivity is not sufficient to reach the method detection limits by direct flow injection, a solid phase extraction clean-up and concentration step is described in Annex C.

PDF Catalog

PDF Pages PDF Title
2 National foreword
7 Foreword
9 1 Scope
2 Normative references
3 Terms and definitions
10 4 Principle
5 Interferences
11 5.1 Biases
5.2 Limitations
6 Reagents and standards
6.1 General
12 6.1.7 Concentrated phosphate-free detergent.
6.2 Preparation of solutions
6.2.3 Stock solution of internal standard substances
13 6.2.4 Internal standard solution (IS1)
6.2.5 Internal standard solution (IS2)
6.2.6 MCYST mix solution (S1)
6.2.7 MCYST mix solution (S2)
6.2.8 MCYST mix solution (S3)
6.2.9 MCYST mix A solution
6.2.10 MCYST mix B solution
6.2.11 MCYST mix C solution
14 6.2.12 MCYST mix D solution
6.2.13 Instrument check mix (high) solution
6.2.14 Calibration control standard (CS1)
6.2.15 Calibration control standard (CS2)
7 Apparatus
7.3 Microsyringes.
15 7.13 Ultrasonic bath
7.15 Liquid chromatograph (LC)
7.17 Mass spectrometer (MS)
8 Sampling
16 9 Procedure
9.1 Preparation of samples
9.1.1 General
9.1.2 Preparation of method blank sample
9.1.3 Preparation of laboratory control spike sample
9.1.4 Preparation of calibration control sample
9.1.5 Preparation of calibration standard solutions
17 9.1.6 Preparation of drinking water and freshwater sample
9.1.7 Sample preparation procedure with freeze/thaw cycles
18 9.2 Instrumental analysis by LC-MS/MS procedure
9.2.1 Instrument set-up parameters
21 9.3 Run processing and quality assurance
9.3.1 Run sequence
9.3.2 Run control operations / limits
22 10 Calibration
23 11 Evaluation and calculation of results
11.1 Identification and calculations
11.2 Calibration curve equation determination
11.3 Internal standard calculation
24 11.4 Internal standard recovery calculation
12 Expressing of results
13 Test report
25 Annex A (informative) Use of high resolution mass spectrometry detectors (HRMS)
27 Annex B (informative) Use of online solid phase extraction coupled to liquid chromatography for the automated analysis of microcystins
33 Annex C (informative) Use of manual solid phase extraction prior to instrumental analysis for improved method detection limits
40 Bibliography

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BS ISO 22104:2021
$167.15