GenX replacement PFOA compound by LC-MS/MS

LC Conditions

Column

Gemini 3 µm C18 110 Å, LC Column 50 x 2 mm, Ea

Brand

Gemini

Part No

00B-4439-B0

Phase Name

C18

Elution Type

Gradient

Mobile Phase

A: 20mM Ammonium Acetate in Water

B: Methanol

Gradient Profile

Step No.

Time(min)

%A

%B

1

0

95

5

2

0.1

45

55

3

4.5

1

99

4

8

1

99

5

8.5

95

5

Flow Rate

0.60 mL/min

Temperature

40°C

System

Shimadzu SCIEX 4500

Detection

LC/MS/MS

Detection Info

Sample Preparation Details

Description

Strata GCB, 500mg/6mL, 30/Pk

Part No

8B-S528-HCH

Sample Pretreatment

All standards including HFPO-DA and its stable isotope labelled surrogate 13C3-HFPO-DA were purchased from Wellington Laboratories (Guelph, Ontario). 200 mL water samples were extracted using Strata®-XL-AW weak anion exchange SPE cartridges following the conditions in the ISO standard 25101. Samples were also passed through Strata GCB following the requirements of DOD QSM 5.1. The final volume of the SPE eluent was 8 mL. Final extracts consisted of 80% methanol and 20% water. Solid Phase Extraction Protocol Cartridge: Strata XL-AW 500 mg/6 mL Part No.: (8B-S051-HCH) Condition: 6 mL 0.3% Ammonium hydroxide in Methanol, followed by 6 mL Methanol Equilibrate: 6mL Water Load: Add sample at about 10 mL/min Note: use an adapter cap (Part no.: AH0-7191) and large volume sample reservoir (Part No.: AH0-7005) Wash: 2x 6mL Water Elute: 10 mL 0.3% Ammonium hydroxide in Methanol(this 10 mL will elute PFAS/GenX analytes) Load: SPE Eluent through Strata GCB 250 mg/6 mL (8B-S528-HCH) Evvaporate: to dryness and reconstitute to 1.0 mL with Methanol/ Water (96:4)(containing internal standards)

Elution 1

Pass Strata XL-AW Eluent through Strata GCB

Evaporation

Evaporate to dryness

Steps

0

Elute

Pass Strata XL-AW Eluent through Strata GCB