18 A Comparison of Assay Techniques for the Analysis of Diarrhetic Shellfish. . .
211
Table 18.1 A comparison of data on DSP toxins in mussel flesh derived from analysis using a
protein phosphatase assay (PP2A) and LC-MS
Method:
PP2A
PP2A
LC-MS
LC-MS
Treatment:
Non-hydrolysed Hydrolysed
Non-hydrolysed Hydrolysed
Site
Date
g OA eq g
1
g OA eq g
1
g OA eq g
1
g OA eq g
1
Inner
07 June 2009 <0:06
0:08
0.02
0.03
Middle 07 June 2009 <0:06
0:12
0.04
0.07
Outer
07 June 2009 <0:06
0:10
0.03
0.04
Inner
05 July 2009
0:19
>0:38
0.18
0.67
Middle 05 July 2009
0:27
>0:38
0.23
0.68
Outer
05 July 2009
0:08
0:26
0.05
0.16
Inner
20 July 2009
0:13
0:30
0.08
0.17
Middle 20 July 2009
0:29
0:37
0.15
0.35
Outer
20 July 2009
0:12
0:28
0.07
0.19
Middle 02 Aug 2009
0:10
0:23
0.05
0.13
Inner
13 Sept 2009 <0:06
0:20
0.01
0.02
Middle 13 Sept 2009 <0:06
0:16
0.00
0.03
Outer
13 Sept 2009
0:09
0:18
0.03
0.05
Inner
08 June 2010 <0:06
0:07
0.02
0.01
Middle 08 June 2010
0:08
0:11
0.01
0.02
Outer
08 June 2010
0:08
0:10
0.02
0.02
Inner
14 June 2010
0:07
0:09
0.00
0.01
Middle 14 June 2010
0:08
0:11
0.01
0.03
Outer
14 June 2010
0:08
0:09
0.03
0.02
Inner
21 June 2010
0:07
0:09
0.00
0.01
Middle 21 June 2010 <0:06
0:09
0.03
0.05
Outer
21 June 2010 <0:06
0:09
0.03
0.05
Inner
28 June 2010 <0:06
<0:06
0.02
0.02
Middle 28 June 2010
0:07
0:14
0.07
0.11
Outer
28 June 2010
0:08
0:13
0.06
0.09
Middle 05 July 2010
0:10
0:14
0.09
0.11
Inner
05 July 2010 <0:06
0:07
0.04
0.04
Outer
05 July 2010
0:09
0:13
0.06
0.09
Inner
09 Aug 2010 <0:06
0:11
0.00
0.01
Middle 09 Aug 2010
0:08
0:15
0.02
0.03
Outer
09 Aug 2010
0:09
0:14
0.05
0.07
Mussel samples were taken from the outer, middle, and inner sites of Killary Harbour indicated
in Fig. 18.1 on various dates in 2009 and 2010. Samples taken in 2009 had been stored frozen for
18 months prior to analysis using both methods. Analysis was carried out on both hydrolysed and
non-hydrolysed extracts
EU official testing method. Commission Regulation (EU) No 15/2011 amending
Regulation (EC) No 2074/2005, established the EU RL LC-MS/MS method as
the reference method for the detection of lipophilic toxins in shellfish for the
purposes of official controls. However, this analytical technique requires expensive
equipment and maintenance as well as highly trained staff to perform routine
211
Table 18.1 A comparison of data on DSP toxins in mussel flesh derived from analysis using a
protein phosphatase assay (PP2A) and LC-MS
Method:
PP2A
PP2A
LC-MS
LC-MS
Treatment:
Non-hydrolysed Hydrolysed
Non-hydrolysed Hydrolysed
Site
Date
g OA eq g
1
g OA eq g
1
g OA eq g
1
g OA eq g
1
Inner
07 June 2009 <0:06
0:08
0.02
0.03
Middle 07 June 2009 <0:06
0:12
0.04
0.07
Outer
07 June 2009 <0:06
0:10
0.03
0.04
Inner
05 July 2009
0:19
>0:38
0.18
0.67
Middle 05 July 2009
0:27
>0:38
0.23
0.68
Outer
05 July 2009
0:08
0:26
0.05
0.16
Inner
20 July 2009
0:13
0:30
0.08
0.17
Middle 20 July 2009
0:29
0:37
0.15
0.35
Outer
20 July 2009
0:12
0:28
0.07
0.19
Middle 02 Aug 2009
0:10
0:23
0.05
0.13
Inner
13 Sept 2009 <0:06
0:20
0.01
0.02
Middle 13 Sept 2009 <0:06
0:16
0.00
0.03
Outer
13 Sept 2009
0:09
0:18
0.03
0.05
Inner
08 June 2010 <0:06
0:07
0.02
0.01
Middle 08 June 2010
0:08
0:11
0.01
0.02
Outer
08 June 2010
0:08
0:10
0.02
0.02
Inner
14 June 2010
0:07
0:09
0.00
0.01
Middle 14 June 2010
0:08
0:11
0.01
0.03
Outer
14 June 2010
0:08
0:09
0.03
0.02
Inner
21 June 2010
0:07
0:09
0.00
0.01
Middle 21 June 2010 <0:06
0:09
0.03
0.05
Outer
21 June 2010 <0:06
0:09
0.03
0.05
Inner
28 June 2010 <0:06
<0:06
0.02
0.02
Middle 28 June 2010
0:07
0:14
0.07
0.11
Outer
28 June 2010
0:08
0:13
0.06
0.09
Middle 05 July 2010
0:10
0:14
0.09
0.11
Inner
05 July 2010 <0:06
0:07
0.04
0.04
Outer
05 July 2010
0:09
0:13
0.06
0.09
Inner
09 Aug 2010 <0:06
0:11
0.00
0.01
Middle 09 Aug 2010
0:08
0:15
0.02
0.03
Outer
09 Aug 2010
0:09
0:14
0.05
0.07
Mussel samples were taken from the outer, middle, and inner sites of Killary Harbour indicated
in Fig. 18.1 on various dates in 2009 and 2010. Samples taken in 2009 had been stored frozen for
18 months prior to analysis using both methods. Analysis was carried out on both hydrolysed and
non-hydrolysed extracts
EU official testing method. Commission Regulation (EU) No 15/2011 amending
Regulation (EC) No 2074/2005, established the EU RL LC-MS/MS method as
the reference method for the detection of lipophilic toxins in shellfish for the
purposes of official controls. However, this analytical technique requires expensive
equipment and maintenance as well as highly trained staff to perform routine