Agricultural Chemicals

The analyses of agricultural chemicals using two columns, RSpak DE-613 and GOLF-413 were performed. The analysis time can be shortened by using RSpak GOLF-413.

Sample :
1. Asulam, 2. Oxine-Cu, MCPP; 2. (Methyl-4-chlorophenoxy)-propionic acid
3. Thiuram, 4. Iprodione ,5. Bensulide, Pencycuron

Column       : Shodex RSpak DE-613 (6.0mmID*150mm)   
Eluent       : 50mM Sodium phosphate buffer(pH3.3)/CH3CN=49/51
Flow rate    : 1.0mL/min
Detector     : UV(0min to 6.9min to 17.0min, 270nm to 243nm to 230nm)
Column temp. : 40deg-C

Column       : Shodex RSpak GOLF-413 (4.6mmID*150mm)
Eluent       : 50mM Sodium phosphate buffer(pH3.2)/CH3CN=48/52
Flow rate    : 1.0mL/min
Detector     : UV(0min to 3.5min to 5.0min, 270nm to 243nm to 230nm)
Column temp. : 40deg-C

Thermally unstable and/or involatile agricultural chemicals which cannot be analyzed by GC or GC/MS can be analyzed by LC/MS.
A semi-micro column RSpak DE-213 was used for the separation.

Sample : 20ng each, 20micro-L
1. Asulam
2. 2-(Methyl-4-chlorophenoxy)-propionic acid, MCPP
3. Thiuram
4. Bensulide, SAP
5. Iprodione
6. Pencycuron

(HPLC)
Instrument   : Agilent 1100
Column       : Shodex RSpak DE-213 (2.0mmID*150mm)
Eluent       : (A): 50mM CH3COONH4 aq.
               (B): CH3CN
               0min to 10min, (B)10% to (B)100%
Flow rate    : 0.2mL/min
Column temp. : 40deg-C

(MS)
Instrument   : Agilent 1100MSD
Mass range   : 105-500(m/z)
Ionization   : Electrospray
Polarity     : Positive, Negative
Fragmentor   : 60V
Nebulizer    : N2(50psi)
Drying gas   : N2(12L/min, 350deg-C)

Nine kinds of Agricultural Chemicals were analyzed by gradient elution with RSpak GOLF-413.

Sample : 20micro-L

1.

10ppm

 Methyl 2-benzo imidazol carbamate, MBC
2.
50ppm
 Asulam
3.
10ppm
 Oxine-Cu
4.
40ppm
 2-(Methyl-4-chlorophenoxy)-propionic acid, MCPP
5.
100ppm
 Thiophanate-Methyl
6.
25ppm
 Thiuram
7.
100ppm
 Siduron
8.
50ppm
 Iprodione
9.
100ppm
 Bensulide, SAP

 

Column       : Shodex RSpak GOLF-413 (4.6mmID*150mm)
Eluent       : (A): 50mM Potassium Phosphate buffer(pH3.0)/CH3CN=90/10, (B): CH3CN
               Step gradient: 0min to 10min, 40%(B), 10min to 30min, 50%(B) 
Flow rate    : 1.0mL/min 
Detector     : Photodiode array(200nm-400nm max.plot)
Column temp. : 40deg-C

Oxine-copper easily makes coordination complex with other metals. When analyzed by an ODS column, the presence of metal-impurity in silica may cause adsorption and/or tailing. The packed gel used in golf course herbicides analysis column, RSpak GOLF-413 is a polymer base. The column does not contain metals thus prevents adsorption of oxine-copper.

Sample : Oxine-Cu, 20micro-L
GOLF-413
ODS
fas
1.152
2.042
 
Columns      : Shodex RSpak GOLF-413,ODS(other manufacturer) (4.6mmID*150mm each)
Eluent       : 20mM H3PO4 aq./CH3CN=95/5
Flow rate    : 1.0mL/min
Detector     : UV(254nm)
Column temp. : 40deg-C