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Polychlorinated Biphenyls in Pond Water
Using 2g 15mL HyperSep C18 Extraction Column
(Part Number: 60108-701)
Sample Preparation
Filter water sample through a 0.45µm filter
Add 2mL of methanol to 200mL of filtered water sample
Mix and degas sample for 2 minutes
Condition C18 Extraction Column
15 to 20mL of hexane
15 to 20mL of methanol
10mL of DI H
2
O
Apply Sample
Load 200mL of sample at a rate of 8 to 10mL/minute
Wash Column
20mL of DI H
2
O
Dry Column
Use maximum vacuum pressure for 20 to 30 minutes
Elute Polychlorinated Biphenyls
20mL of hexane
Concentration/Evaporation
Evaporate to dryness under a nitrogen stream at room
temperature
Injection/Analysis
Reconstitute with 100µL of methanol and inject 1 to 2µL
aliquot onto GC column
Pesticides Extracted
Aroclor 1026
Aroclor 1221
Aroclor 1232
Aroclor 1242
Aroclor 1248
Aroclor 1254
Aroclor 1260
LC/MS/MS Analysis of Phenoxyacetic Acid Herbicides
Using 10g 75mL HyperSep C18 Extraction Column
(Part Number: 60108-703)
Sample Preparation
Collect 10 to 100 grams of soil sample
Add DI H
2
O to form a slurry
Mix for 15 minutes
Adjust pH to 2 using 50% aq H
2
SO
4
Filter sample through previously acidified filter media
Condition HyperSep C18 Extraction Column
1 x 5mL CH
3
OH
1 x 5mL DI H
2
O
NOTE:
Do not allow the cartridge to dry out
Apply Sample
Load sample at 10mL/minute
Elute Phenoxyacetic acid Herbicides
2 x 5mL CH
3
OH
Collect at 1 to 2mL/minute
Evaporate to dryness at <40°C using N
2
Analysis
Reconstitute in 100µL of mobile phase
Inject 10 to 100µL onto LC/MS
Mobile phase: 0.1 M ammonium acetate (A):methanol (B)
% B
Time
25
0
60
15
Compound
+ve Ion
m/z
-ve Ion
m/z
Dalapon
141
Dicamba
238
184
2,4-D
238
184
MCPA
218
199
Dichloroprop
252
235
MCPP
232
213
2,4,5-T
272
218
2,4,5-TP Silvex
286
269
Dinoseb
228
240
2,4-DB
266
247
2,4-D, butoxy ethanol ester
321
185
2,4-T, butoxy ethanol ester
372
195
2,4,5-T, butoxy ethanol ester
328
195
2,4-D, ethyl hexyl ester
350
161
Recommended HPLC Columns
Part Number
ODS-Hypersil C18 5µm, 100 x 2mm
30105-102130
MOS2-Hypersil C18 3µm, 100 x 2mm
30303-102130
Environmental
Applications