Page 63 - Application Notebook - Solution for Food Safety

Application No.C104
News

8:817.50 > 255.20(-) 400 8:817.50 > 255.20(-) 8:817.50 > 255.20(-) 8:817.50 > 255.20(-) 8000 8:817.50 > 255.20(-) 8:817.50 > 255.20(-) 90000 8:817.50 > 255.20(-) 8:817.50 > 255.20(-)
300 D-1 375 D-1 900 D-1 4000 D-1 7500 D-1 40000 D-1 D-1 400000 D-1
350 7000 80000
275 350000
325 800 3500 6500 35000
250 70000
300 6000
700 30000 300000
225 275 3000 5500
60000
200 250 600 5000 25000 250000
225 2500 4500 50000
175
200 500 4000 200000
150 2000 20000
175 3500 40000
400
125 150 3000 150000
1500 15000 30000
100 125 300 2500
100 2000 100000
75 1000 10000 20000
75 200 1500
50
50 500 1000 5000 50000
100 10000
25 500
25
0 0 0 0 0 0 0 0
-25 -500
8.0 9.0 8.0 9.0 8.0 9.0 8.0 9.0 8.0 9.0 8.0 9.0 8.0 9.0 8.0 9.0
0.025 ɹɹɹɹɹɹɹɹ 0.1 0.5 1 5 10 50 ng/mL
0.05
Fig. 3 MRM Chromatograms of Dinophysistoxin 1 (DTX1)
In addition, the calibration curves of OA and DTX1 are shown in Fig. 4. In both cases, the coefficient of determination
R was greater than 0.9999, indicating excellent linearity. Comparable linearity was also obtained for the other four
2
substances.
Thus, instrumental analysis of shellfish by LC/MS/MS offers high sensitivity and accuracy, making it a highly effective
analytical method. For this reason it is attracting attention as an alternative to the traditional MBA method.
Area (×1,000,000) Area (×1,000,000)
OA 2.25 DTX1
2.25
0.025-50 ng/mL (n=3) 2.00 0.025-50 ng/mL (n=3)
2.00
1.75
1.75
1.50
1.50
1.25 1.25
1.00 1.00
0.75 0.75
0.50 0.50
2
R = 0.9999153 R = 0.9999308
2
0.25 0.25
R = 0.9999577 R = 0.9999654
0.00 0.00
0 10 20 30 40 50 0 10 20 30 40 50
Concentration Concentration
Fig. 4 Calibration Curves of OA and DTX1
Table 2 Analytical Conditions
Column : InertSustain C8 (50 mm L. × 2.1 mm I.D., 3 μm)
Mobile Phases : A 2 mmol/L Ammonium Formate – Water (pH adjusted to 8.5 with ammonia water)
: B Methanol
Time Program : 20 %B (0 min) – 100 %B (10 min) – 20 %B (10.01 min) – STOP (15 min)
Flowrate : 0.2 mL/min
Column Temperature : 40 ˚C
Injection Volume : 10 μL
Probe Voltage : +4.0 kV/-3.0 kV (ESI-positive / negative mode)
DL Temperature : 200 ˚C
Block Heater Temperature : 400 ˚C
Interface Temperature : 350 ˚C
Nebulizing Gas Flow : 3 L/min
Drying Gas Flow : 10 L/min
Heating Gas Flow : 10 L/min
MRM Transition : (+) PTX6 906.50 > 835.40, PTX1 892.60 > 821.40, PTX2 876.50 > 805.40
: (-) OA 803.50 > 255.20, YTX1 1141.50 > 1061.30, DTX1 817.50 > 255.20
The diarrhetic shellfish toxin standards were provided courtesy of Dr. Toshiyuki Suzuki of the Japanese National Research Institute of Fisheries Science.
Reference 1: July, 2014, Food Safety Commission of Japan "Natural Poison Evaluation Report – Okadaic Acid Group Among Bivalves"
http://www.fsc.go.jp/fsciis/evaluationDocument/list?itemCategory=009

First Edition: Apr. 2015

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