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Environmental

dissociation (CID) is used to generate the frag­

ment ions. CID spectra for paraquat and diquat

Table 1

MRM tra nsitions and MS cond it ions used to generate

C10 spectr a for paraquat and diquat.

are shown in Figures 2 and 3. This approach has

Precursor Ion

FragmentIons

DP

CollisionEnergy

been used in many pharmaceutical and environmlz

l!!lill

leV)

Paraquat [Ml+-

W]

170a

40

30

mental applications, to generate unmatched limits

18S

169b

of detection or quantification, precision, and accu­

Paraquat-d8 [M " - D' ]

178a

40

30

racy. For accurate quantification, we used

193 (int. std.)

par aqu at-dS and diquat-d4 as internal standards

Diquat [ M -

W]

157a

35

30

"

(Table

1),

to compensate for matrix effects and to

183

168b

Diquat·d4 [M " - D' ]

158a

35

30

~(

int.

std

.)

Figure 2

CIOspect ra for paraquat" at CE

==

25eV.

a -

MRM

transition

185/ 170

used for quantification

b - MRM

transition185/169 used for confirmation

[M"-H']

, ', n:

b

I~

corr ect for random and systematic errors in sepa­

ration and detection.

For trip licate injections of 8 concentrations of ana­

lytes in deioni zed water and in lake water, from

5f-lg/lOOmL to 100f-lg/100mL for paraquat and

from

O.lf-

lg/lOOmL to 100f-lg/lOOmL for diquat,

correlation coefficients for calibration curves were

>0.995, using a linear fit and

1/x

weighting factor.

These results indicat e that quantification can be

perfo rmed with good linearity and sensitivity.

Minimum detection limits (MDL) for the method,

for paraquat and diquat in deionized water, were

5f-lg/L and 0.1ug/L, respectively.

LC/MS is a powerful tool for analyses of challenging

environmental contaminants. In LC/MS analyses of

paraquat and diq uat, the combination of an

Applied Biosystems API 3200™mass spectrometer

and an Ultra Quat HPLC column ensures fast, sen­

sitive, and accurate results.

Figure 3

CIOspect ra for diquat' at CE

==

25eV.

a -

MRM

transition 183/ 157 used for quantification

b - MRM

transition183/ 168 used for confirmation

[M"-H']

a

1'-

b

II I

.,

, ••

~.

s

»

"

.

...., ,, " " .""

. "

,

" ).'"' .

.., .

" .... "n'

free

literature

Simple, SensitiveHPLC/UV Analysis for Paraquat and DiquatUsing High-Recovery Solid Phase

Extractionand anUltra Quat HPLC Column

These highly charged quaternary amines are poorly retained onalkyl stationary phases. Using only

acetonitrile,water, and a solvation-blockingreagent, our separationsystemalters theinteractions

among analyte, mobile phase, and stationary phase, and promotessolubility of theanalytesin the

stationary phase. In oursystem, the detection limit is 6ppb for either herbicide, andtheanalysis is

completed in less than 10 minutes. An optimized solid phase extractioncartridge concentratesthe

herbicides for theanalysis. lit. cat.# 580006

Environmental HPLC: Applications-Columns-ReferenceMaterials

Restek HPLCcolumnssupportenvironmental HPLCapplicationswith rapid analysis times and effec­

tive analyte resolution. Sample turn-around canbe50%faster, or more, thanwith alternative columns.

Inaddition, weprepare analytical reference materialsand sample clean-up products for thesemeth­

ods. Applications in thispublication include polyaromatic hydrocarbons, carbamates, phenoxyacid her­

bicides,explosives, carbonyls, and paraquatldiquat. lit. cat.# 5974lA

2006.03

• 15 •

Reference

L

Simple, SensitiveHPLCIUVAnalysis for ParaquatandDiquat, Using

High-Recovery Solid Phase Extraction andanUltra QuatHPLCColumn

Applications Note580006, RestekCorporation, Feb. 2006.

Reference availablefrom Restekon request.

Ultra Quat Columns & Guard Cartridges

Spm Column, 4.6mm

cat.

#

price

~50mm

9181565

$399

150mm(withTrident'" Inlet Fitting)

9181565-700 $414

UltraQuat Guard cartridge".s'--:::c::-::-:=:-::--:::c:-::_

10

x

2.1mm

918150212 $131

10

x

4.Omm

918150210

$131

20x 2.1mm

918150222

$131

20x 4.Omm

918150220

$131

Paraquat & Diquat Calibration Mix

diquat dibromide

paraquat dichloride

1,000/-lg/mL

each inwater,

l mt/ arnpul

cat.

#

32437 (ea.) $26

free

literature

HPLC Essentials

GenuineRestekReplacement Parts will keep your Agilent,

Beckman,Hitachi, PerkinElmer, Shimadzu, ThermoSeparation

Products,orWaters systemrunning smoothly and chromatogra­

phy sharp. Restek parts equal or exceed theperformanceof

original components. lit. cat.# 59012A

800-356- 1688 ·

www.restek.com

Website :

www.chromtech.net.au

E-mail :

info@chromatech.net.au

TelNo : 03 9762 2034 . . . in AUSTRALIA