Detection of Ziram by LC/APCI/MS Hiroshi MORIWAKI Osaka City Institute of Public Health &...
-
Upload
peter-hamilton -
Category
Documents
-
view
219 -
download
0
Transcript of Detection of Ziram by LC/APCI/MS Hiroshi MORIWAKI Osaka City Institute of Public Health &...
Detection of Ziram by LC/APCI/MS
Hiroshi MORIWAKI
Osaka City Institute of Public Health & Environmental Sciences
Ziram
Zn2+
S
S-N
CH3
CH3S
S-
NH3C
H3C
((CH3)2NCS.S)2ZnM.W. 305.8m.p. 240Log Pow 1.09
use pesticideantifouling agent
toxicity endocrine disruptormutagencarcinogen
Analysis of Ziram
Direct detection by GC/MS → ×
Conventional method
Decomposition of the ligand to CS2
Chemical speciation of dithiocarbamate pesticides ×
LC/MS ( Direct detection of ziram )
Ionization
ESI/MS
Positive ion mode Negative ion mode
× ×
×
×APCI/MS
○
Corona current<0.6A
Corona current>0.6A
Ion mode
A)
B)
Mass spectrum
05000000
1000000015000000
2000000025000000
3000000035000000
40000000
0 1 2 3 4 5 6
Corona current (A)
Pea
k in
tens
ity
Corona current vs. peak intensity
05000000
1000000015000000200000002500000030000000350000004000000045000000
0 10 20 30 40 50
Cone voltage (V)
Pea
k in
tens
ity
Cone voltage vs. peak intensity
Ionization APCI positive ionizationAPCI probe temperature 400 ℃
source temperature 120 ℃capillary voltage 3.0 kVcorona current 1.5 Acone voltage 20 V
desolvation gas flow rate 250 lhr-1 (N2)
Conditions of APCI/MS
column Tosoh TSK-GEL -25002.0× 150mm
mobile phase MeOHflow rate 0.2ml/mincolumn temprature 30℃
Column separation
Mass chromatogram
0
2000
4000
6000
8000
10000
12000
14000
16000
18000
0 5 10 15 20 25
Conc. (g/ ml)
Pea
k in
tens
ity
Calibration curve
Summary
・ Direct detection of Ziram by LC/APCI/MS・ Corona current > 0.6A・ LC separation: GPC column
・ Instrumental detection limit: 2mg/L
Next step
・ Development of the pretreatment・ Use of LC/MS/MS
ref. H. Moriwaki, Y. Yamaguchi and M. Fukushima:Rapid Commun. Mass Spectro., in press (2001).