78
Table 22: Relative recoveries [%] of selected sPCA/mPCA compounds and the internal standards 13 Ci 0 -
rra/rv-chlordane, octachloronaphthalene (OCN) and MC8 (a chlordane congener). Extraction as well as a
stepwise and complete clean-up of spiked sea sand and sediments were tested (spiked amount 1.5-2.5 pg
of sPCA (55.5 % Cl) or 1.5-20 pg of mPCA (52 % Cl) mixture). ECNI was employed for quantification.
No.
13^
'-'10“
trans-
Chlordane
C 10 H 16 C1
6
CnH 18 Cl 6
Recovery in %
C n H 17 Cl 7 C 12 H 20 C1 6
Ci 2 H 19 Cl 7
Ci 3 H 22 Cl 6
Extraction (matrix: sea sand)
l a
84
101
105
na
91
116
2 a
78
96
97
na
90
na
98
Extraction (matrix: sodium sulphate)
1
69
na
97
78
82
78
na
2
64
na
100
81
101
85
na
3
74
93
88
84
93
96
97
Adsorption chromatography with Florisil®
r
88
na
101±9*
109±11*
109±12*
109±12*
na
2
75
na
82
82
81
86
na
3
88
na
90
87
84
96
na
Clean-up (matrix: sea sand)
1
75
73
81
na
75
101
na
2
69
54
63
na
60
71
na
3
73
79
78
na
86
94
na
4
76
97
89
na
101
115
na
Recovery in %
13 C
!io-trans-
C 14 H 24 C1 6
Ci 5 H 26 Cl
6 C 14 H 23 C1 7 c 15 H 25 ci 7
Chlordane
Extraction (matrix: sea sand) 8
1 75 92
2 61 87
3 62 85
Adsorption chromatography with Florisil®
1 77 103
2 89 84
3 86 104
Clean-up (matrix: sea sand)
1 72 84
2 83 87
93
96
97
94
90
98
89
91
100
114
107
117
92
88
97
99
104
115
86
81
79
50
82
82
Recovery in %
Nr. 13 C 10 -trans- OCN MC8 C 10 H 16 C1 6 C n H 17 Cl 7 C 14 H 24 C1 6 C 15 H 26 C1 6
Chlordane
Matrix: North Sea sediment UE 67/GAUSS 349
1
72
85
-
0
0
0
0
2 C
77
87
82
120
95
57
71
3 d
72
88
73
84
81
117
126
4 e
67
82
79
120
112
90
114
Matrix
: North Sea sediment BL2/GAUSS 387
1
80
74
74
0
0
0
0
2 C
77
93
74
105
102
168
197
a) without copper, b) 5000 ng sPCA with 55,5 % Cl, c) with 500 ng sPCA and 500 ng mPCA, d) with
1000 ng sPCA and 1000 ng mPCA, e) with 1500 ng sPCA and 1500 ng mPCA, * 5 parallel
measurements
na: not analysed
