LA180-E008

SHIMADZU APPLICATION NEWS

● GAS CHROMATOGRAPHY
No. G214
Analysis of Pesticides in Agricultural Products using
ECD-2010 or FPD-2010
As of 13 March 2002, the Japanese Food Hygiene detected in raw or frozen imported vegetables and in
Laws prescribe limits for 229 pesticides. However, domestically grown fruits and vegetables have focused
faced with the problems of residual pesticides in interest on the analysis of pesticides.
imported vegetables, the Ministry of Health, Labour This Application News presents examples of the
and Welfare plans to expand the scope of these analysis of frequently detected organochlorine and
regulations to cover 400 pesticides by 2006. Reports organophosphorus pesticides.
of levels of pesticides exceeding these limits

■ Analysis of 13 Organochlorine Pesticides using ECD-2010

Intensity α-BHC

γ-BHC

chlorfenapyr
450000

captafol
400000

] deltamethrin
β-BHC

] cyhalothrin
captan
350000
δ-BHC

EPN
300000

] fenvalerate
250000

] cypermethrin
200000

] permethrin
150000

100000

50000

0
0 10 20 30 40
min

Fig. 1 Chromatogram of 13 Organochlorine Pesticides by ECD-2010 (1µL splitless injection of 100ppb standard solution)

Fig. 1 shows the chromatogram of a mixed standard

solution containing 13 organochlorine pesticide Table 1 Minimum Detectable Quantities (absolute value/s)
components (100ppb acetone solution). Fig. 2 shows Minimum detectable Per second (fg/s)
the calibration curve for each component. Table 1 quantity (fg)
shows the minimum detectable quantities (absolute α-BHC 26 8
values) determined from the results in Fig. 1 and the β-BHC 50 12
minimum detectable quantity per second, determined γ-BHC 28 8
by dividing the minimum detectable quantity by the δ-BHC 39 9
corresponding peak width. (Note: These values are captan 60 15
not guaranteed as they may change according to the chlorfenapyr 29 8
analytical conditions (column and detector etc. captafol 66 18
conditions)). EPN 51 13
cyhalothrin 71 21
2500000 permethrin 262 71
cypermethrin 249 65
2000000
α-BHC fenvalerate 121 33
Peak Area

1500000 chlorfenapyr deltamethrin

captan
92 22
1000000 cyhalothrin Note: For components with isomers, the main peak was used for the
permethrin calculations.
500000

0
0 20 40 60 80 100
Conc (ppb)

2500000 2500000

2000000 2000000
γ-BHC δ-BHC
Peak Area

Peak Area

1500000 1500000
captafol β-BHC
EPN deltamethrin
1000000 1000000
fenvalerate cypermethrin
500000 500000

0 0
0 20 40 60 80 100 0 20 40 60 80 100
Conc (ppb) Conc (ppb)

Fig. 2 Linearity of Calibration Curves

No.G214

■ Analysis of 11 Organophosphorus Pesticides using FPD-2010 (P-mode)

Intensity

dichlorvos

methamidophos

tolclofos-methyl

parathion-methyl

parathion
350000

chlorpyrifos

malathion
300000

dimethoate
acephate
250000

200000

phenthoate

EPN
150000

100000

50000

0 10 20 30
min

Fig. 3 Chromatogram of 11 Organophosphorus Pesticides by FPD-2010 in P-mode (2µL splitless injection of 90ppb standard solution)

Fig. 3 shows the chromatogram of a mixed standard corresponding peak width. (Note: These values are
solution containing 11 organophosphorus pesticide not guaranteed as they may change depending on the
components (90ppb acetone solution). Fig. 4 shows analytical conditions (column and detector etc.
the calibration curve for each component. Table 2 conditions)).
shows the minimum detectable quantities (absolute Table 2 Minimum Detectable Quantities (absolute value/s)
values) determined from the results in Fig. 3 and the
minimum detectable quantity per second, determined Minimum detectable Per second (pg/s)
quantity (pg)
by dividing the minimum detectable quantity by the
dichlorvos 10.1 3.6
methamidophos 17.6 4.0
1.8E+07 acephate 27.7 7.3
1.6E+07 dimethoate 18.2 5.4
1.4E+07
tolclofos-methyl 19.2 6.1
1.2E+07 methamidophos
Peak Area

1.0E+07 acephate
parathion-methyl 22.0 6.4
8.0E+06 chlorpyrifos chlorpyrifos 20.1 6.0
EPN
6.0E+06 malathion 27.1 8.5
4.0E+06
parathion 9.9 3.1
2.0E+06
phenthoate 30.7 9.4
0.0E+00
0 0.5 1 EPN
Conc (ppm)
33.5 10.4

1.8E+07 1.8E+07
1.6E+07 1.6E+07
1.4E+07 1.4E+07
1.2E+07 parathion 1.2E+07
Peak Area

Peak Area

dichlorvos
1.0E+07 dimethoate 1.0E+07
tolclofos-methyl
8.0E+06 parathion-methyl 8.0E+06
malathion
6.0E+06 phenthoate 6.0E+06
4.0E+06 4.0E+06
2.0E+06 2.0E+06
0.0E+00 0.0E+00
0 0.5 1 0 0.5 1
Conc (ppm) Conc (ppm)

Fig. 4 Linearity of Calibration Curves

Table 3 Analytical Conditions for Fig. 1 Table 4 Analytical Conditions for Fig. 3
(Organochlorine Pesticides) (Organophosphorus Pesticides)

Model : GC-2010, ECD-2010 Model : GC-2010, FPD-2010

Column : Rtx-1 Column : DB-1301
30m × 0.25mmI.D. df=0.25µm 30m × 0.25mmI.D. df=0.25µm
Column Temp : 50˚C (1min) → 120˚C at 20˚C/min Column Temp : 50˚C (1min) → 120˚C at 20˚C/min
→ 300˚C at 5˚C/min → 280˚C at 5˚C/min
Injection Temp : 250˚C Injection Temp : 250˚C
Detector Temp : 330˚C Detector Temp : 280˚C
Carrier Gas : He 150kPa Carrier Gas : He 150kPa
Detector : ECD (Makeup Gas : N2 30mL/min) Detector : FPD (H2: 80mL/min, Air: 120mL/min)
Injection : Splitless 1µL Injection : Splitless 2µL

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