! (xct) !#$%&'( - chemical analysis, life sciences, and … · · 2017-05-312a...
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�� !" /�� (XCT)�� !"#�� !"#$%&'(
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Bernhard Wüst, Christian Sauber
Agilent Technologies GmbH,
Hewlett-Packardstr. 8, 76337
Waldbronn
Germany
Hans (J.) A. van Rhijn
RIKILT -Institute of Food Safety
Bornsesteeg 45,6700 AE Wageningen
the Netherlands
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�� /�� /�� !"#$%&'( 1100 XCT��
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�� !"#$%&'(MRM)��� NBA-AMOZ �
NBA-AOZ�� !"#$%&'(
NBA-SEMSEM
NBA-AHDAHD
NBA-AMOZ
NBA-AOZ
AMOZ
AOZ
ON+
O_
ON
N
N
OO
O
O N N
N
N
O
OO
O
O
O
N
HN
NOO
N
O
OH2N
ON+
O_
O N
O
ON
N
N
OO
O
H2N
ON
N
NO
O
O
N
NO
NH2
HN
OO
ON+
NO
O_
O
NH2
HN
H2N
O
NHON+
O_
ON N
N
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NH
H2NO
NH2
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� 1�� !"��� !"# , � 5 mL � 0.2 M �
�� !"#$%�� !50�� !"#$%&'
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��500��0.3 M�� !"#$%&�� 2 M�
�� !"#$ pH�� ! 7��� 4 mL�� �
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�� !"#$�� !"#"$%&'()*��
�� !"�� ��500-µL��� �50 mL��
80 mL�� 0.5 mL�� !"�� !"# $% .
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2
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�� (Biosolve, 13683502)
���32% (Merck, 100319)
2-�� !"(2-NBA) (Sigma, N6001)
12�� !"#$ (Merck, 106578)
�� ! (Merck, 106498)
��� (Biosolve, 05402602)
�� (Merck, 10063)
�� (Biosolve, 01203502)
�� !�99.5% (Aldrich, 15.193-9)
�� /�� /�� !"�� !"#(HPLC): Agilent 1100
�� �! : 0.4 mL/min
�� : Zorbax XDB-C8, 2.1 mm x 50 mm, 3.5 m
�� : A: H2O + 0.1% ��
B: �� + 0.1% ����: 0-14 min; 10% A -45% A; 14-16 min; 45% A -90% A
�� ! : 500 l �� !" 50 l
1100 LC/MSD XCT �� !"�� ! : ESI �� !"
�� !" : 45 psi
�� !" : 12 L/min
�� !" : 350 �
�� !(Skimmer): 20 V
�� !"#$: 55 V
�� !"( Trap Drive): 55
ICC: on
�� !"#$(MRM)
4 �� !": 0-2.2 min, 2.2-7.4 min, 7.4-10.6 min, 10.6-13.9 min
�� 1: �� !": �� !" , �� !"
�� 2: m/z 335 �MS/MS, Isolation width: 2.0, Cut-off: 140, Amplitude: 1.16
m/z 340 �MS/MS, Isolation width: 2.0, Cut-off: 140, Amplitude: 1.16
�� 3: m/z 209 �MS/MS, Isolation width: 2.0, Cut-off: 140, Amplitude: 1.28
m/z 249 �MS/MS, Isolation width: 2.0, Cut-off: 140, Amplitude: 1.25
�� 4: m/z 236 �MS/MS, Isolation width: 2.0, Cut-off: 140, Amplitude: 1.25
m/z 240 �MS/MS, Isolation width: 2.0, Cut-off: 140, Amplitude: 1.25
�� !
NBA-AMOZ: EIC of 261 + 291 (m/z 335 � MS/MS), �� !: 4.5 min
NBA-dAMOZ: EIC of 266 + 296 (m/z 340 � MS/MS), �� !: 4.5 min
NBA-SEM: EIC of 166 + 192 (m/z 209 � MS/MS), �� !: 9.9 min
NBA-AHD: EIC of 134 (m/z 249 � MS/MS), �� !: 10.0 min
NBA-AOZ: EIC of 134 (m/z 236 � MS/MS), �� !: 10.8 min
NBA-dAOZ: EIC of 134 (m/z 240 � MS/MS), �� !: 10.8 min
Max Acc time: 150 ms
Smart target: 100000
Scan: 100-350
3
NBA-AMOZ2A 2B
123
x104
0
NBA-SEM
x104
0.0
0.4
0.8
1.2
2 4 6 8 10 12 Time [min]
NBA-d5AMOZ
NBA-AMOZ
NBA-d5AMOZx105
0.0
0.4
0.8
NBA-AHD
0
2000
4000
6000
NBA-AOZ
x104
0.0
1.0
2.0
NBA-d4AOZ
NBA-SEM
NBA-AHD
NBA-AOZ
NBA-d4AOZ
x104
0.0
1.0
2.0
122.9
133.8
148.8158.9
166.7176.8
204.8 222.8 239.9
264.9
295.9
192.9 261.9
290.9
317.8 333.9
135.8148.7
165.7
190.8 207.8217.8 228.7
120.8
133.8
138.7144.8
162.7
170.7188.7
200.7212.8
230.7248.8
119.9
133.8
148.8
164.7
171.8190.7
206.7
217.7 235.8
0246
x104
x104
x104
x104
IntensityIntensity
0
1
2
3
02000400060008000
02000400060008000
0.0
1.0
2.0
0.0
1.0
2.0
3.0
100 125 150 175 200 225 250 275 300 325 m/z
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4
0
1000
2000
3000
4000
2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0
Time [min]
Inte
nsity
1.0
0.8
0.6
0.4
0.3
0.0
0.00 0.25 0.50 0.75 1.00 1.25
Relative concentratiion
Rel
ativ
e re
spon
se
1.0
0.8
0.6
0.4
0.3
0.0
ISTD R
esponse x10 6
1.50 1.75 2.00 2.25 2.50
�� !"#$%&'()*+),-./.012
�� !�� !"#$%&'(�� 3 � 4��
� 3. �� !"#$NBA-AMOZ�� !"# 0.125 g/kg
� 4. �� NBA-AMOZ, �� !"# , 0.125 g/kg-2 g/kg�� !"#$%�� !
5
NBA-d4 AOZ
x104
0.0
0.4
0.8
1.2
NBA-AOZ
x104
0.00
0.50
1.00
1.50
NBA-AHD
10000
20003000400050006000
NBA-d5 AMOZ
x104
0
2
4
6
NBA-AMOZ
0
1
2
3
4
x104Intensity
NBA-SEMx104
01234
2 4 6 8 10 12 Time [min]
�� NBA-AMOZ� NBA-SEM��� !"!#$%
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��NBA-AMOZ: 0.125 µg/kg�NBA-AOZ�NBA-SEM:
0.25 µg/kg� NBA-ADH: 0.5 µg/kg��� !"#$
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6
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www.agilent.com/chem
� 1. �� !"#$%&'()*+,-./()012
NBA-SEM NBA-AOZ NBA-AMOZ NBA-AHDStandard Accuracy % Accuracy % Accuracy % Accuracy %( g/kg) SD % (average) SD % (average) SD % (average) SD % (average)0.125 3.77 98.81 2.29 98.94 4.34 101.10
0.25 2.26 102.72 2.52 101.76 5.87 95.55 6.05 98.31
0.5 3.40 100.72 3.35 100.58 6.21 105.19 4.59 103.87
1 3.56 96.62 3.01 101.90 5.46 99.11 6.53 100.22
2 2.94 101.12 2.13 96.82 5.77 99.05 6.97 97.60
All calibration curves linear weighted 1/x n = 6
7
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5989-0738CHCN
www.agilent.com/chem
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