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Choosing a QuEChERS dSPE Sorbent
Primary and secondary amine exchange material (PSA) is the base sorbent used for QuEChERS dSPE cleanup of fruit and vegetable
extracts because it removes many organic acids and sugars that might act as instrumental interferences. In addition, C18 or graphi-
tized carbon black (GCB) may be used to remove lipids or pigments, respectively. Choice of sorbent should be based on matrix
composition and target analyte chemistry. Most methods make specific recommendations for acidic, basic, and planar pesticides,
which may require additional considerations.
As seen in Table II, GCB can have a negative effect on the recoveries of certain pesticides that can assume planar shapes (e.g. chlo-
rothalonil and thiabendazole). The work shown here was done with 50 mg GCB per mL extract, which emphasizes this effect. The
EN 15662 QuEChERS method recommends less GCB, which improves recoveries of planar pesticides, but still assures the removal
of pigments that can degrade GC-MS performance. To simplify and speed up sample prep, Restek QuEChERS tubes are available in
the sorbent combinations and amounts specified by EN 15662 and AOAC methods.
Sorbent Guide
Sorbent
Removes
PSA*
sugars, fatty acids, organic acids, anthocyanine pigments
C18
lipids, nonpolar interferences
GCB**
pigments, sterols, nonpolar interferences
*PSA—primary and secondary amine exchange material
**GCB—graphitized carbon black
Table II:
Select sorbents based on matrix and target analyte chemistry.
(Percent recovery using C18 or GCB, relative to PSA alone).
Rt (min)
pesticide
CAS Number
action/use
classification
C18*
GCB**
9.50
dichlorvos
62-73-7
insecticide
organophosphorus
111
116
9.67
methamidophos
10265-92-6
insecticide
organophosphorus
105
107
11.75
mevinphos
7786-34-7
insecticide
organophosphorus
112
130
12.02
o
-phenylphenol
90-43-7
fungicide
unclassified
106
97
12.14
acephate
30560-19-1
insecticide
organophosphorus
128
147
13.89
omethoate
1113-02-6
insecticide
organophosphorus
120
119
14.74
diazinon
333-41-5
insecticide
organophosphorus
108
127
14.98
dimethoate
60-51-5
insecticide
organophosphorus
124
151
15.69
chlorothalonil
1897-45-6
fungicide
organochlorine
125
13
15.86
vinclozolin
50471-44-8
fungicide
organochlorine
102
98
16.21
metalaxyl
57837-19-1
fungicide
organonitrogen
105
117
16.28
carbaryl
63-25-2
insecticide
carbamate
114
111
16.60
malathion
121-75-5
insecticide
organophosphorus
124
160
16.67
dichlofluanid
1085-98-9
fungicide
organohalogen
122
103
17.51
thiabendazole
148-79-8
fungicide
organonitrogen
88
14
17.70
captan
133-06-2
fungicide
organochlorine
88
91
17.76
folpet
133-07-3
fungicide
organochlorine
108
63
18.23
imazalil
35554-44-0
fungicide
organonitrogen
115
95
18.39
endrin
72-20-8
insecticide
organochlorine
104
101
18.62
myclobutanil
88671-89-0
fungicide
organonitrogen
119
114
19.07
4,4-DDT
50-29-3
insecticide
organochlorine
102
95
19.22
fenhexamid
126833-17-8
fungicide
organochlorine
118
77
19.40
propargite 1
2312-35-8
acaricide
organosulfur
110
95
19.43
propargite 2
2312-35-8
acaricide
organosulfur
121
114
19.75
bifenthrin
82657-04-3
insecticide
pyrethroid
106
81
20.04
dicofol
115-32-2
acaricide
organochlorine
98
54
20.05
iprodione
36734-19-7
fungicide
organonitrogen
118
90
20.21
fenpropathrin
39515-41-8
insecticide
pyrethroid
113
96
21.32
cis
-permethrin
52645-53-1
insecticide
pyrethroid
106
65
21.47
trans
-permethrin
51877-74-8
insecticide
pyrethroid
109
71
23.74
deltamethrin
52918-63-5
insecticide
pyrethroid
97
52
*50 mg PSA, 50 mg C18, **50 mg PSA, 50 mg GCB
% recovery = RRF C18 or GCB X 100
RRF PSA
Strawberry extracts were spiked at 200 ng/mL with pesticides and subjected to dSPE with PSA only. Results were used to generate single point calibration curves. Spiked extracts
were then subjected to additional dSPE sorbents (either C18 or GCB). Results are shown as percent recoveries relative to PSA alone.
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