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This document is the Intellectual Property of SGS AXYS Analytical Services Ltd. and contains Proprietary and Confidential Business <br />Information. It may not be reproduced or distributed without written permission of the owner. © SGS AXYS Analytical Services Ltd, 2020. <br />SGS AXYS Analytical Services Ltd, 2045 Mills Road W., Sidney, BC, Canada, V8L 5X2. Tel. (250) 655-5800, fax (250) 655-5811. <br />This is not a controlled document; it is subject to change without notification. <br /> <br />SGS AXYS Analytical Services Ltd. <br /> <br />MSU-110 Rev 14, 28-May-2020 Summary of MLA-110 Rev 02 Ver 07 Page 4 of 23 <br />SGS AXYS confidential, not to be distributed without written permission <br />Tissue sample size may be up to 2 g. After addition of isotopically labelled surrogate standards <br />the sample is extracted with methanolic potassium hydroxide solution, with acetonitrile, and finally <br />with methanolic potassium hydroxide solution, each time collecting the supernatants. The <br />supernatants are combined, treated with ultra pure carbon powder and evaporated to remove <br />methanol. The resulting solution is diluted with water and cleaned up by solid phase extraction <br />(SPE) on a weak anion exchange sorbent. The eluate is spiked with recovery standards and <br />analyzed by LC-MS/MS. <br />All AFFF samples are pre-screened before analysis to determine the appropriate amount of <br />sample to analyze. A suitable subsample is dissolved in water, spiked with surrogate standards <br />and extracted by solid phase extraction (SPE). The extracts are treated with carbon powder, <br />spiked with recovery standards and analyzed by LC-MS/MS. <br />Blood, Serum sample size may be up to 2 mL. After the addition of isotopically labelled surrogate <br />standards the sample is extracted with 50% formic acid. The resulting solution is cleaned up by <br />solid phase extraction (SPE) on a weak anion exchange sorbent. The eluent tubes are spiked <br />with recovery standards and then eluent collected and analyzed by LC-MS/MS. <br />2.0 INSTRUMENTATION <br />Analysis of the sample extract is performed on a UPLC (ultrahigh performance liquid <br />chromatography) reversed phase C18 column using a solvent gradient. The column is coupled to <br />a triple quadrupole mass spectrometer run at unit mass resolution in the Multiple Reaction <br />Monitoring (MRM) in negative electrospray ionization mode. <br />3.0 CALIBRATION <br />Initial calibration of the LC-MS/MS instrument is performed by the analysis of five or more calib- <br />ration solutions. A mid-level calibration standard is analyzed to verify the initial calibration and <br />injected after: <br />• at least every 12 hours. <br />• For DoD accredited work after every 10 client samples or every 12 hours, whichever occurs <br />first, and at the end of the instrumental run sequence. <br /> <br /> <br /> <br />Nominal Concentrations of Calibration Solutions (ng/mL) <br /> CAL A* CAL B CAL C CAL D CAL E <br />(CAL-VER) CAL F CAL G CAL H <br />Perfluoroalkyl carboxylates <br />PFBA 0.2 0.4 0.8 2 10 50 250 1000 <br />PFPeA 0.1 0.2 0.4 1 5 25 125 500 <br />PFHxA 0.05 0.1 0.2 0.5 2.5 12.5 62.5 250 <br />PFHpA 0.05 0.1 0.2 0.5 2.5 12.5 62.5 250 <br />www.axysanalytical.com <br />Page 9 of 94