• Application Note

Emerging Contaminant of Concern - Perfluorinated Compounds (PFOS/PFOA)

Emerging Contaminant of Concern - Perfluorinated Compounds (PFOS/PFOA)

  • Waters Corporation

This is an Application Brief and does not contain a detailed Experimental section.

Abstract

Recent research has provided evidence that perfluorinated compounds (PFCs), such as perfluorooctanesulfonic acid (PFOS) and perfluorooctanoic acid (PFOA), are persistant organic pollutants and are ubiquitous in the environment.

Benefits

Analytical method for perfluorinated compounds (PFCs)

Introduction

Recent research has provided evidence that perfluorinated com-pounds (PFCs), such as perfluorooctanesulfonic acid (PFOS) and per-fluorooctanoic acid (PFOA), are persistant organic pollutants and are ubiquitous in the environment. Because PFCs may be toxic and have bioaccumulative properties, there is growing interest in the develop-ment of analytical methods for PFCs in the environment.

Experimental

UPLC conditions

Instrument:

ACQUITY UPLC System

Column:

ACQUITY UPLC BEH C18, 1.7 μm, 2.1 x 50 mm,

Flow Rate:

0.40 mL/min

Injection Volume:

10 μL [full loop injection mode]

Column Temp:

40 ˚C

Mobile Phase:

A: 20 mM ammonium acetate in water/acetonitrile [90:10]

B: Methanol/acetonitrile [60:40]

Gradient:

15% – 95% B over 8 minutes

Curve:

Linear

MS conditions

Instrument:

Quattro Premier XE

Ionization Mode:

ESI -

Capillary Voltage:

3 kV

MS Mode:

MRM

Desolvation Temp:

350 ˚C

Source Temp:

150 ˚C

PFC

MRM Transition

Cone (V)

Collision (eV)

PFBS

299>80

40

30

PFOS

499>80

50

40

C3

163>119

20

13

C4

213>169

15

10

C5

263>219

15

9

C6

313>269

15

12

C7

363>319

15

10

C8

413>369

15

10

C9

463>419

15

10

C10

513>469

15

10

C11

563>519

15

10

C12

613>569

15

10

Optimized MRM transition parameters.

UPLC-MS/MS of 12 PFCs spiked at 10 μg/kg in chicken liver.
Oasis WAX Sorbent and SPE protocol for water and tissue.

Sample preparation

Method 1: Water

Water samples [100 mL] were spiked with the appropriate com-pounds, adjusted to pH 3 with formic acid, and then processed by SPE. The SPE eluate [Elute 2] was collected in polypropylene test tubes, diluted with 2 mL of 2% aqueous formic acid and brought to 5 mL with water. Alternatively, the eluate may be evaporated and reconstituted in mobile phase prior to analysis, but polypropylene labware should be used exclusively.

Method 2: Tissues

A 1 mL aliquot of supernatant was diluted to 20 mL with water and the pH was adjusted to 4–5 using 2% formic acid. This solution was then loaded on an Oasis WAX cartridge. SPE eluates were evapo-rated and reconstituted in 1 mL of mobile phase [polypropylene labware].

Results and Discussion

Recovery from Drinking Water [%]

Spike Level μg/L

C11

PFBS

PFOS

C3

C4

C5

C6

C7

C8

C9

C10

0.1

101

122

109

108

119

97

184

107

83

121

101

0.3

94

110

117

95

132

105

110

119

126

137

118

0.7

119

102

98

91

107

93

118

100

78

103

126

1

117

113

94

128

106

98

130

100

88

100

110

4

84

104

86

101

99

99

102

102

92

115

99

10

101

104

100

98

101

100

87

89

82

103

99

Recovery of PFCs from drinking water.

References

  1. Environmental System Solutions 720001601EN
  2. Analysis of Perfluorinated Compounds (PFCs) on the ACQUITY UPLC System and the Quattro Premier XE in ES-MS/MS 720001761EN
  3. Separation of Branched PFOS Isomers by UPLC with MS/MS Detection 720001694EN
  4. Oasis WAX Sorbent for UPLC/MS Determination of PFOS and Related Compounds in Water and Tissue 720001817EN
  5. Analysis of Perfluorinated Compounds using UPLC and MS/MS Detection 720001848EN

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