SHIMADZU APPLICATION NEWS LAAN-A-G-E005

GAS CHROMATOGRAPHY No.G216 Analysis of Residual Pesticides in Agricultural Products using ECD-2010 (Part 2)

Lately, public concern regarding the safety of food G214 of the Application News, we focused on products has become extremely heightened due to the pesticides that are often detected in imported problem of pesticide residues on imported vegetables vegetables and domestic vegetables. In this issue, we and unregistered pesticides being used domestically. will introduce some fundamental data regarding Given this situation, the Ministry of Health, Labour and organochlorine pesticides that are among the 244 Welfare of Japan is expected to expand to 714 the pesticides currently regulated, other than the number of agricultural chemicals regulated with substances addressed in the previous issue. respect to their content in food products. In issue

Intensity

140000

130000

120000

110000 pp'-DDE 100000

90000

80000 op'-DDT pyrifenox Z 70000 pyrifenox E trifluralin dichlofluanid 60000

50000

40000 bifenthrin 30000 ] fluvalinate acrinathrin chlorobenzilate 20000 halfenprox

10000

0 -5000

0 10 20 30 40 50 min

Fig.1 Chromatogram of 11 Organochlorine Pesticides detected by ECD-2010 (1µL splitless injection of 10ppb standard solution)

Intensity

140000

130000

120000

110000 aldrin 100000 dieldrin tefluthrin 90000 pp'-DDT pp'-DDD bifenox

80000 endrin

70000

60000

50000 folpet

40000

30000 tralomethrin

20000 ] flucythrinate

10000 ] cyfluthrin

0 -5000

0 10 20 30 40 50 min

Fig.2 Chromatogram of 11 Organochlorine Pesticides detected by ECD-2010(1µL splitless injection of 10ppb standard solution) No.G216

Table 1 lists the minimum detectable quantities (absolute values) obtained from the results in Fig.1 and 2, and the minimum detectable quantities per 400000 second, which was calculated by dividing each 350000 300000 aldrin minimum detectable quantity by the corresponding 250000 bifenox pyrifenox Z peak width. 200000 trifluralin

Peak Area 150000 tralomethrin Note: These values could vary depending on analytical 100000 halfenprox conditions (column and detector status, etc.), so 50000 0 they are not guaranteed values. 0 12345678910 Conc (ppb) The calibration curves for each substance are shown in Fig.3.

400000 350000 Table 1 Minimum Detectable Quantities 300000 dieldrin pp'-DDT 250000 MDQ (fg) MDQ per Second (fg/s) op'-DDT 200000 folpet

acrinathrin 115 38 Peak Area 150000 chlorobenzilate aldrin 24 7 100000 cyfluthrin bifenox 36 11 50000 0 bifenthrin 74 23 01 23 456 789 10 Conc (ppb) chlorobenzilate 116 29 cyfluthrin 183 54 dichlofluanid 45 14 dieldrin 19 6 endrin 29 9 flucythrinate 157 50 400000 fluvalinate 103 32 350000 folpet 57 16 300000 pp'-DDE 250000 halfenprox 136 41 tefluthrin 200000 pyrifenox E op'-DDT 31 9 bifenthrin

Peak Area 150000 pp'-DDD 30 9 100000 acrinathrin pp'-DDE 19 6 50000 0 pp'-DDT 30 9 012345678910 pyrifenox E 48 14 Conc (ppb) pyrifenox Z 41 11 tefluthrin 23 8 tralomethrin 86 25 trifluralin 35 12

Note: The primary peak was used for calculating 350000

substances containing isomers. 300000 pp'-DDD 250000 endrin 200000 dichlofluanid 150000 fluvalinate flucythrinate Peak Area 100000

50000

0 345678910 012 Conc (ppb)

Fig.3 Linearity of Calibration curves

Table 2 Analytical Conditions for Fig.1 and 2

Model : GC-2010, ECD-2010 Column : Rtx-1 30m × 0.25mm I.D. df =0.25µm Column Temp : 50ûC(1min)-20ûC/min-120ûC -5ûC/min-300ûC Injection Temp : 250ûC Detector Temp : 330ûC Carrier Gas : He 150kPa (Constant Pressure) Detector : ECD (Makeup Gas : N2 30mL/min) Injection : Splitless 1µL

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