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Trichothecenes Appendix 1.

Methods for screening for B-trichothecenes and particularly for deoxynivalenola

Referenceb

Matrix

Amount of sample
(g)

Extraction

Clean-up

Technique

Malone et al. (1998)

Wheat, barley, maize, bran, oats

25

CH3CN/H2O

Mycosep

Fluorometric determination after derivatization

Trucksess et al. (1987)

Corn, wheat, barley

50

CH3CN:H2O: MeOH (70:25:5) 200ml, shake 60 min

Carbon column C18 column

TLC fluorodensitometric

Trucksess et al. (1984)

Wheat, maize

50

CH3CN/H2O

Charcoal/ alumina/celite

TLC

Fernandez et al. (1994)

Wheat

50

CH3CN/H2O

Charcoal/ alumina/ celite

TLC

Eppley et al. (1986)

Wheat

50

CH3CN/H2O

Charcoal/ alumina/celite

TLC

Eppley et al. (1984)

Wheat

50

CH3CN/H2O

Charcoal/ alumina

TLC

Romer (1986)

Foods, feeds

 

CH3CN/H2O

Charcoal/ alumina

TLC

Romer (1999)
AccutoxTM

 

 

Distilled water

 

ELISA

Xu et al. (1988)

Wheat, maize

 

CH3CN/H2O

None

ELISA (acetylated)

Ridascreen™
DON (2000)

Cereals, feeds

2

CH3CN/H2O

 

ELISA

(acetylated)

Sinha et al. (1995)

Wheat, maize

1

MeOH/ H2O

 

ELISA

Abouzied (2000)

Cereals

NA

H2O

None

ELISA

Veratox™ (1998)

Wheat

10

H2O

None

CD-ELISA

Corn

Barley

Oat

Schneider et al. (2000)

Wheat

10

CH3CN/H2O

None

ELISA (IgY)

Mills et al. (1990)

Wheat

NA

60% MeOH

None

ELISA

Usleber et al. (1992)

Wheat

2

MeOH/ H2O

Ethyl acetate

ELISA

Referenceb

Matrix

Toxins assayed

LOD/LOQ
(ng/g)

Spiking levels
(ng/g)

Recovery
(%)

CV
(%)

Malone et al. (1998)

Wheat, barley, maize, bran, oats

DON

100

500–50 000

NA

NA

Trucksess et al. (1987)

Corn, wheat, barley

DON

NA

200

81–88

2–20

NIV

 

100

78–89

 

FX

 

50

61–108

 

Trucksess et al. (1984)

Wheat, maize

DON

20/40

100–1000

85–93

3–17

(wheat)

(wheat)

 

 

20/100

100–1000

77–80

6–12

(maize)

(maize)

 

 

Fernandez et al. (1994)

Wheat

DON

40/NA

200

83

NA

 

400

82

 

 

800

72

 

Eppley et al. (1986)

Wheat

DON

50/NA

50

90

30–87

 

100

96

 

 

300

95

 

 

1000

78

 

Eppley et al. (1984)

Wheat

DON

NA/200

200–5000

80

NA

Romer (1986)

Foods, feeds

DON

300/NA

900–1100

99

8

NIV

500/NA

750–1100

92

15

FX

300/NA

900–1100

99

9

Romer (1999)
AccutoxTM

 

DON

 

500

 

 

Xu et al. (1988)

Wheat, maize

DON

NA

10–1000

102

12

 

 

100

15

Ridascreen™
DON (2000)

Cereals, feeds

DON

1.25/NA

NA

80–90

 

3-AcDON

 

 

 

 

15-AcDON

 

 

 

 

Sinha et al. (1995)

Wheat, maize

DON

250/NA

NA

NA

NA

15-AcDON

 

 

 

 

Abouzied (2000)

Cereals

DON

20/NA

NA

NA

NA

Veratox™ (1998)

Wheat

DON

300/500

NA

NA

NA

Corn

Barley

Oat

Schneider et al. (2000)

Wheat

DON

160/NA

525

104-120

6

Mills et al. (1990)

Wheat

DON

100/NA

NA

NA

NA

Usleber et al. (1992)

Wheat

DON

4.5 ng/ml/200

200–1000

71–79

3.6–4.9

a For definitions of abbreviations, see end of Trichothecenes Appendix 6.

b The references are listed in the monograph on deoxynivalenol.

 

Trichothecenes Appendix 2.

Quantitative methods for B-trichothecenes and particularly for deoxynivalenola

Referenceb

Matrix

Amount of sample (g)

Extraction

Clean-up

Technique assayed

Veldman et al. (1992)

Feed

20

CH3CN/H2O

Celite/cahrcoal/ aluminium oxide

HPLC–UV

Rajakylä et al. (1987)

Wheat, rye

20

CH3CN

Bond Elut

HPLC–MS

Zabe et al. (2000)

Food

NA

NA

Immunoaffinity

HPLC–NA

Josephs et al. (1998)

Wheat

1

SFE

SFE

GC–ECD

Pineiro et al. (1996)

Liquid culture

50

MeOH

SPE–C18

HPLC–UV

Sano et al. (1987)

Maize, wheat, barley

20

CH3CN/H2O

Florisil and CN-

HPLC–FLD

Sep Pak

(methyl acetate)

Schuhmacher et al. (1996)

Wheat

15

CH3CN/H2O

Mycosep

HPLC–DAD

Berger et al. (1999)

Wheat

10

CH3CN/H2O

Mycosep 227, 216

LC–MS

Cahill et al. (1999)

Wheat

50

H2O/PEG

DONtest

HPLC–UV

Razzazi-Fazeli et al. (1999)

Wheat

25

CH3CN/H2O

Mycosep

HPLC–

APCI–MS

Reutter (1999)

Cereals, feed

25

CH3CN/H2O

Charcoal/ alumina/ celite/Iimmuno-affinity column

HPLC–UV

Mulders et al. (1986)

Cereals

25

CHCl3/EtOH

Silica gel

GC–ECD (HFB)

GC–MS (HFB)

Scott & Kanhere (1986)

Cereals

50

CH3OH/H2O

Silica gel

GC–ECD (TMS)

Tacke & Casper (1996)

Wheat, barley, malt

5

CH3CN/H2O

C18/alumina

GC–ECD (TMS)

Weingärtner et al. (1997)

Wheat

25

CH3CN/H2O

MycoSep‘

GC–ECD (TMS/TBT)

Schollenberger et al. (1998)

Cereals, food, feed

10

CH3CN/H2O

Florisil/Bond Elut CBA

GC–MS (TFA)

Croteau et al. (1994)

Maize

50

CH3CN/H2O, shake 2.5 h

Charcoal/ alumina

GC–ECD (DMAP, HFBA)

Adler et al. (1992)

Wheat

20

MeOH/ H2O

Silica gel/C18

GC–ECD (TMS)

Blaas et al. (1984)

Cereals

20

MeOH/ H2O, hexane

Florisil

GC–MS (TMS)

Seidel et al. (1993)

Wheat, maize

10

MeOH/ H2O

Florisil/C18

GC–ECD (HFB)

van Egmond (2000)

Wheat

25

CH3CN/H2O

Mycosep

GC–FID

Young & Games (1993)

Liquid culture

NA

NA

NA

SFC–UV

SFC–MS

Groves et al. (1999)

Maize

5

CH3CN/H2O

Aluminium oxide/C18

GC–MS (TMS)

Petterson (1992)

Barley, oats, wheat

20

CH3CN/H2O

Charcoal/ aluminia

GC–ECD (TMS)

Stenwig et al. (1992)

Barley, oats

50

CH3CN/H2O

Charcoal/ aluminia/ celite

GC–ECD (TMSI)

Lauren & Agnew (1991)

Maize

20

CH3CN/ MeOH/H2O

Alumina/ cation resins/celite

HPLC–UV

GC–ECD (TFAA)

Scudamore et al. (1998)

Maize

30

CH3CN/4% KCl

Charcoal/ aluminia

GC–MS (TFAA)

Mirocha et al. (1998)

Wheat, barley

25

CH3CN/H2O

C18/alumina

GC–MS (TMSI, TCMS)

Liu et al. (1997)

Wheat, barley,oats

 

CH3CN/H2O

Charcoal/ aluminia/ celite

GC–ECD (TMSI)

Park et al. (1991)

Cereals

50

CH3CN/H2O

Florisil

GC–MS (TMI/TMA/ TMCS)

Tanaka et al. (1986)

Wheat, barley

20

CH3CN/H2O

Florisil/C18

GC–ECD

(TMS)

Swanson et al. (1986)

Milk

40 mL

Chem tube/ ethyl acetate

C18

GC–ECD (TMS, HFB)

Dahlem et al. (1986)

Urine

9 mL

Clin-Elut/ethyl acetate

 

GC–ECD (TMS)

Faeces

12 g

MeOH/H2O/ Clin-Elut

C18

 

Kiessling et al. (1984)

Rumen fluid

5 mL

MeOH/0.1% NaCl

C18

GC–FID

Scott et al. (1993)

Beer

50 mL

Chem-Elut/ ethyl acetate/ MeOH

C18

GC–MS

(HFB)

 

Tanaka et al. (1990)

Cereals

50

CH3CN/H2O

Florisil

GC–ECD

(TMS)

Scott & Trucksess (1997)

Wheat, maize

NA

NA

Charcoal/C18

GC–MS

(TMS, HFB)

Scott et al. (1989)

Wheat

50

MeOH/ H2O

C18/alumina/ carbon

GC–ECD

(HFB, TMS)

Luo et al. (1990)

Wheat, maize

40

CH3CN/H2O

Florisil

GC–ECD

(TMS)

Möller & Gustavsson (1992)

Cereals

50

CH3CN/ EtOAc/H2O

Florisil-Sep Pak

GC–ECD

(Tri-syl/

TBT)

Onji et al. (1998)

Cereals

15

CH3CN/H2O

Bond Elut florisil

GC–MS

(on-column)

Krska et al. (1997)

Wheat

25

CH3CN/H2O

Mycosep

GC–ECD

(Tri-syl/TBT)

Krska (1998)

Wheat

25

CH3CN/H2O

Mycosep

GC–ECD

(Tri-syl/TBT)

Josephs (1999)

Wheat

25

CH3CN/H2O

Mycosep

GC–ECD

(Tri-syl/

TBT)

Kotal et al. (1999)

Cereals

5

CH3CN/H2O CH3CN/ MeOH

GPC (BioBeads S-X3)

GC–ECD

(TFAA)

Referenceb

Matrix

Amount of sample
(g)

Toxins
ng/g

LOD/LOQ
levels

Spiking
(%)
(ng/g)

Recovery

CV
(%)

Veldman et al. (1992)

Feed

20

DON

100–500/NA

500–600

60–86

NA

Rajakylä et al. (1987)

Wheat, rye

20

DON

250–1000/NA

NA

75

10

Zabe et al. (2000)

Food

NA

DON

NA

0–5

80

NA

Josephs et al. (1998)

Wheat

1

DON

1600/5350

2350–16 750

53

9.6

Pineiro et al. (1996)

Liquid culture

50

DON

NA

NA

96

NA

Sano et al. (1987)

Maize, wheat, barley

20

DON

20/NA

1000

> 70

NA

NIV

 

 

 

 

FX

 

 

 

 

Schuhmacher et al. (1996)

Wheat

15

DON

500/2000

1000–50 000

79

9.6

Berger et al. (1999)

Wheat

10

DON

6/50

NA

86

3.6

FX

3/40

 

91

3.4

3-AcDON

3/25

 

98

2.6

Cahill et al. (1999)

Wheat

50

DON

100/NA

100–10 000

100–81

NA

Razzazi-Fazeli et al. (1999)

Wheat

25

DON

NA/40

50–500

86

3.5–7.7

NIV

NA/50

 

70

 

Reutter (1999)

Cereals, feed

25

DON

NA/50

NA

NA

NA

 

NA/100

 

 

 

Mulders et al. (1986)

Cereals

25

DON

20/NA

100

99

11

Scott & Kanhere (1986)

Cereals

50

DON

20/NA

200

121

NA

 

 

1000

93 (barley)

 

Tacke & Casper (1996)

Wheat, barley, malt

5

DON

50/NA

500–20 000

94–100

 

Weingärtner et al. (1997)

Wheat

25

DON

35/123

100–2000

102

9.5–18

3-AcDON

41/143

 

96

 

15-AcDON

35/123

 

95

 

FX

35/124

 

97

 

NIV

33/117

 

66

 

Schollenberger et al. (1998)

Cereals, food, feed

10

DON

7/23

50–500

83–98

NA

FX

6/21

 

82–120

 

15-AcDON

7/22

 

73–108

 

3-AcDON

5/16

 

88–110

 

NIV

12/38

 

71–107

 

Croteau et al. (1994)

Maize

50

DON

NA/50

100

73

NA

 

 

250

108

 

 

 

1000

81

 

Adler et al. (1992)

Wheat

20

DON

NA

NA

NA

NA

Blaas et al. (1984)

Cereals

20

DON

10/NA

NA

NA

NA

NIV

 

 

 

 

Seidel et al. (1993)

Wheat, maize

10

DON

3.5/NA

NA

75–80

5

van Egmond (2000)

Wheat

25

DON

25/75

300

96

4.8

NIV

 

 

96

3.8

FX

 

 

98

2.9

3-AcDON

 

 

102

0.7

Young & Games (1993)

Liquid culture

NA

DON

150/NA

NA

NA

NA

3-AcDON

100/NA

 

 

 

ZEN

250/NA

 

 

 

Groves et al. (1999)

Maize

5

DON

500/NA

1000

80–100

NA

NIV

 

 

 

 

FX

 

 

 

 

3-AcDON

 

 

 

 

15-AcDON

 

 

 

 

Petterson (1992)

Barley, oats, wheat

20

DON

10/NA

NA

NA

NA

NIV

 

 

 

 

Stenwig et al. (1992)

Barley, oats

50

DON

10/NA

NA

90

NA

Lauren & Agnew (1991)

Maize

20

DON

30/NA

NA

55–70

NA

NIV

20/NA (GC)

 

73–103

 

 

 

 

 

 

Scudamore et al. (1998)

Maize

30

DON

10/NA

100

72–80

10–16

NIV

10/NA

 

 

 

FX

10/NA

 

 

 

Mirocha et al. (1998)

Wheat, barley

25

DON

NA

1 000

97

NA

 

 

5 000

88

 

 

 

10 000

87

 

Liu et al. (1997)

Wheat, barley,oats

 

DON

30/NA

NA

NA

11

 

3-AcDON

30/NA

 

 

 

NIV

50/NA

 

 

Park et al. (1991)

Cereals

50

DON

15/NA

1000

83

NA

NIV

 

 

89

 

Tanaka et al. (1986)

Wheat, barley

20

DON

2/NA

NA

NA

NA

NIV

 

 

 

 

Swanson et al. (1986)

Milk

40 mL

DON

1 ng/mL/NA

2.5–10 ng/mL

82

10

Dahlem et al. (1986)

Urine

9 mL

DON

50/NA

200–5000 ng/mL

86

8.5

Faeces

12 g

 

 

 

87

10

Kiessling et al. (1984)

Rumen fluid

5 mL

DON

2/NA

NA

43

NA

Scott et al. (1993)

Beer

50 mL

DON

1.5 ng/mL

5–20 ng/mL

103

NA

NIV

0.3 ng/mL

 

90

 

ZEN

2 ng/mL/NA

 

97

 

Tanaka et al. (1990)

Cereals

50

DON

2/NA

300

88

1.9–11

NIV

2/NA

300

88

 

ZEN

1/NA

500

91

 

Scott & Trucksess (1997)

Wheat, maize

NA

DON

7–100/NA

500–1000

81–96

NA

NIV

 

500–1000

48–73

 

Scott et al. (1989)

Wheat

50

DON

20–50/NA

200–1000

81–108

NA

NIV

200/NA

200–1000

71–102

 

Luo et al. (1990)

Wheat, maize

40

DON

5/NA

200

97–103

NA

NIV

5/NA

200

 

 

Möller & Gustavsson (1992)

Cereals

50

DON

NA

25–250

86–111

NA

NIV

 

 

72–110

 

FX

 

 

84–95

 

3-AcDON

 

 

91–106

 

Onji et al. (1998)

Cereals

15

DON

100–500/NA

60

75

22

FX

 

 

49

29

3-AcDON

 

 

82

28

Krska et al. (1997)

Wheat

25

DON

NA

100–2000

96

9.5

Krska (1998)

Wheat

25

DON

40/NA

100–2000

96

9.5

Josephs (1999)

Wheat

25

DON

28/57

257–2060

103

4.3–7.8

NIV

41/82

204–1438

76

 

FX

28/56

280–2240

106

 

3-AcDON

23/47

255–2040

107

 

15-AcDON

23/46

280-2240

107

 

Kotal et al. (1999)

Cereals

5

DON

NA/50

2000

88

NA

NIV

NA/40

 

87

 

FX

NA/100

 

78

 

a For definitions of abbreviations, see end of Trichothecenes Appendix 6.

b For references, see the monograph on deoxynivalenol.

 

Trichothecenes Appendix 3.

Methods for screening for A-trichothecenes and particularly for T-2 and HT-2 toxinsa

Referenceb

Matrix

Amount of sample
(g)

Extraction

Clean-up

Technique

Romer (1986)

Foods, feeds

 

CH3CN/H2O

Charcoal/ alumina

TLC

Kawamura et al. (1990)

Cereals

20

CH3CN/H2O

Florisil

icELISA

Märtlbauer et al. (1991)

Milk

NA

MeOH

None

ELISA

Barna-Vetro et al. (1997)

Cereals

 

89% CH3CN

None

ELISA

Yang & Luo (2000)

Wheat

20

CHCl3/EtOH

Charcoal/ alumina

ELISA

Referenceb

Matrix

Amount of sample
(g)

Toxins assayed

LOD/LOQ
(ng/g)

Spiking
levels
(ng/g)

Recovery
(%)

CV
(%)

Romer (1986)

Foods, feeds

 

T-2

500(TLC)/NA

850-1200

98

12

HT-2

 

 

 

13

Kawamura et al. (1990)

Cereals

20

T-2

0.2/NA

NA

NA

NA

Märtlbauer et al. (1991)

Milk

NA

T-2

0.5/NA

NA

68-98

5-20

Barna-Vetro et al. (1997)

Cereals

 

T-2

50/NA

NA

85

3-15

Yang & Luo (2000)

Wheat

20

T-2

NA

NA

NA

NA

From Hack (1994), Gendloff (1987), and Hunter (1985), with sensitivities of 5 pg/ml (0.25 pg/assay), 10 ng/ml (0.5 ng/assay), and 50 ng/assay, respectively. Park & Chu (1996) reported the efficiency of ELISA and RIA for the analysis of T-2 toxin and of 3-AcDON in naturally contaminated maize samples. A homogeneous competition inhibition immunoassay for T-2 toxin was reported by Ligler et al. (1987).

a For definitions of abbreviations, see end of Trichothecenes Appendix 6.

b For references, see monograph on T-2 and HT-2 toxins

Trichothecenes Appendix 4.

Quantitative methods for A-trichothecenes and particularly for T-2 and HT-2 toxinsa

Referenceb

Matrix

Amount of sample (g)

Extraction

Clean-up

Technique

Berger et al. (1999)

Wheat

10

CH3CN/H2O

Mycosep 227, 216

LC–MS

Rajakylä et al. (1987)

Wheat, rye

20

CH3CN

Bond Elut

HPLC–MS

Möller & Gustavsson (1992)

Cereals

50

CH3CN/ EtOAc/H2O

Florisil-Sep Pak

GC–ECD (Tri-syl/ TBT)

Rosen & Rosen (1983)

Maize

10

MeOH

Silica gel/C18

GC–MS

Schollenberger et al. (1998)

Cereals, food, feed

10

CH3CN/H2O

Florisil/Bond Elut CBA

GC–MS (TFA)

Onji et al. (1998)

Cereals

 

CH3CN/H2O

Bond Elut florisil

GC–MS (on-column)

Croteau et al. (1994)

Maize

50

CH3CN/H2O, shake 2.5 h

Charcoal/ alumina

GC–ECD (DMAP, HFBA)

Plattner et al. (1989)

Cultures

 

Ethyl acetate

charcoal

GC–MS (Tri-syl/TBT)

Scott & Kanhere (1986)

Standards

NA

NA

NA

GC–ECD (TMS, HFB)

Groves et al. (1999)

Maize

5

CH3CN/H2O

Aluminium oxide/C18

GC–MS (TMS)

Petterson (1992)

Barley, oats, wheat

20

CH3CN/H2O

Charcoal/ alumina

GC–ECD (TMS)

Scudamore et al. (1998)

Maize

30

CH3CN/4 KCL

Charcoal/ alumina

GC–MS (TFAA)

Hietaniemi & Kumpulainen (1991)

Cereals, feed

20

MeOH/ H2O

Silica gel/ Florisil/C18

GC–MSD (TMSI)

Park et al. (1991)

Cereals

50

CH3CN/H2O

Florisil

GC–MS (TMI/TMA/ TMCS)

Kiessling et al. (1984)

Rumen fluid

5 mL

MeOH/0.1% NaCl

C18

GC–FID (?)

Scott (1997)

Wheat, maize

NA

NA

Charcoal/C18

GC–MS (TMS, HFB)

Scott et al. (1989)

Wheat

50

MeOH/ H2O

C18/alumina/ carbon

GC–ECD (HFB, TMS)

Luo et al. (1990)

Wheat, maize

40

CH3CN/H2O

Florisil

GC–ECD (TMS)

Josephs (1999)

Wheat

25

CH3CN/H2O

Mycosep

GC–ECD (HFBI)

Kotal et al. (1999)

Cereals

5

CH3CN/H2O

GPC (Bio Beads S-X3)

GC–ECD (TFAA)

CH3CN/MeOH

 

HT-2

Referenceb

Matrix

Amount of sample (g)

Toxins assayed

LOD/LOQ
(ng/g)

Spiking levels (ng/g)

Recovery
(%)

CV
(%)

Berger et al. (1999)

Wheat

10

T-2

3/60

 

87

4.6

HT-2

1/10

 

90

1.7

Rajakylä et al. (1987)

Wheat, rye

20

T-2

250–1000/NA

NA

89

6.3–7.7

HT-2

 

 

90

 

Möller & Gustavsson (1992)

Cereals

50

T-2

NA

250–2500

76–93

NA

 

HT-2

 

 

71–94

Rosen & Rosen (1983)

Maize

10

T-2

20/50

111

80

14

HT-2

5/20

46

91

8.7

Schollenberger et al. (1998)

Cereals, food, feed

10

T-2

2/6

50–500

87–110

NA

HT-2

5/18

 

74–109

 

Onji et al. (1998)

Cereals

 

T-2

100–500/NA

60

98

22

Croteau et al. (1994)

Maize

50

T-2

NA/100

100

70/121

NA

HT-2

NA/50

250

NA/95

 

 

 

1000

83/99

 

Plattner et al. (1989)

Cultures

 

T-2

NA

NA

NA

NA

Scott & Kanhere (1986)

Standards

NA

T-2

NA

NA

NA

NA

HT-2

 

 

 

 

Groves et al. (1999)

Maize

5

T-2

500/NA

1000

80–100

NA

HT-2

 

 

 

 

Petterson (1992)

Barley, oats, wheat

20

T-2

50/NA

NA

NA

NA

HT-2

10/NA

 

 

 

Scudamore et al. (1998)

Maize

30

T-2

10/NA

100

0–103

20–38

HT-2

10/NA

100

21–53

 

DAS

10/NA

100

64–73

 

Hietaniemi & Kumpulainen (1991)

Cereals, feed

20

T-2

15/NA

NA

72–130

NA

 

HT-2

 

 

 

Park et al. (1991)

Cereals

50

T-2

15/NA

1000

83

NA

Kiessling et al. (1984)

Rumen fluid

5 mL

T-2

10/NA

NA

67

NA

HT-2

5/NA

NA

NA

 

Scott (1997)

Wheat, maize

NA

T-2

NA

4000

94

NA

HT-2

 

1200–2400

88–93

 

Scott et al. (1989)

Wheat

50

T-2

400/NA

200–4000

66–91

NA

HT-2

100–200/NA

200–4000

72–110

 

Luo et al. (1990)

Wheat, maize

40

T-2

100/NA

200

97–103

NA

HT-2

100/NA

200

 

 

Josephs (1999)

Wheat

25

T-2

10/37

51–1027

100

2.2

HT-2

10/38

52–1047

117

 

Kotal et al. (1999)

Cereals

5

T-2

NA/200

2000

91

NA

NA/100

 

105

 

 

a For definitions of abbreviations, see end of Trichothecenes Appendix 6.

b For references, see monograph on T-2 and HT-2 toxins

Trichothecenes Appendix 5.

Analytical methods used in surveys summarized in Appendix A of the monograph on
deoxynivalenol and Appendices A and B of the monograph on T-2 and HT-2 toxinsa

Referenceb

Matrix

Amount of sample (g)

Extraction

Clean-up

Method of quantification

Toxins assayed

LOD/ LOQ (ng/g)

Spiking levels
(ng/g)

Recovery
(%)

RSDr

RSDR

Abouzied et al. (1991)

Grain foods

25

CH3CN:H2O
9:1

 

ELISA

DON

1000

 

 

 

 

Ali et al. (1998)

Maize

20

CH3CN:H2O
3:1
100 ml

Florisil column

GC–MS

DON

10/NA

 

 

 

 

TMS derivatives

NIV

10/NA

 

 

 

 

Eskola et al. Cereals (2000a,b)

 

 

Mycosep 227

GC–MS
column

DON

NA/10

 

 

 

 

 

TMS derivatives

3-AcDON

 

 

 

 

 

NIV

 

 

 

 

 

FX

 

 

 

 

 

DAS

 

 

 

 

 

HT-2

NA/20

 

 

 

 

T-2

NA/20

 

 

 

 

FAO/WHO (2000)

Cereals

20

H2O 8 ml

Petroleum ether:ethanol: H2O

TLC

 

 

 

 

 

 

 

Cereal products

 

Chloroform+ ethanol (8+2)
100 ml

 

 

 

 

 

 

 

 

Fernández et al. (1994) (modified from Trucksess et al., 1984)

Wheat

50

CH3CN:H2O
84:16
200 ml

Charcoal/celite/ alumina column

HPTLC
Chloroform:
acetone:2-
propanol
8:1:1

DON

40/NA

200

83

 

 

 

 

400

82

 

 

 

 

800

72

 

 

Furlong & Valente Soares (1995)

Wheat, maize, wheat products

 

Methanol:4%
KCl 9:1

Chloroform

GC–FID

DON

200/NA

 

85

 

 

Charcoal/celite/ alumina column

HFB
derivatives

NIV

100/NA

 

87

 

 

DAS

100/NA

 

83

 

 

T-2

100/NA

 

87

 

 

HT-2

500/NA

 

91

 

 

T-2 triol

300/NA

 

 

 

 

T-2 tetrol

400/NA

 

 

 

 

Golinski et al. (1996)

Wheat

20

Tanaka et al. (1985)

Tanaka et al. (1985)

HPLC
C-R4A C-18
column UV
(229 nm)
methanol
water 20%

DON

10/NA

 

 

 

 

NIV

 

 

 

 

 

Groves et al. (1999)

Maize, maize products

5

CH3CN:H2O
84:16, 20 ml
shake 60 min

Mixture of neutral aluminum oxide and C-18 packing material

GC–MS
TMS
derivatives

17 toxins

500/NA

1000

80–100

 

 

Hietaniemi & Kumpulainen (1991)

Grains, feeds

20

CH3CN:H2O 95:5, 100 ml, homogenize 5 min

Hexane isobutanol Silica gel column
Florisil or Sep Pak C18 column

GC–MS

DON

5

 

72–128

 

 

TMS derivatives

DAS

5

 

(mean, 100)

 

 

3-AcDON

5

 

 

 

 

FX

5

 

 

 

 

NIV

5

 

 

 

 

T-2

15

 

 

 

 

HT-2

15

 

 

 

 

Home Grown Cereals Authority (1999, 2000)

Wheat

20

CH3CN:H2O
84:16, 100 mL
shake 120 min

Mycosep No.
225 column

GC–MS

DON

20/NA

 

 

 

 

TMS derivatives

T-2

20/NA

 

 

 

 

HT-2

20/NA

 

 

 

 

Kamimura et al. (1981)

Maize

100

CH3OH:H2O
95:5, 200 mL
shake 30 min

1-Amberlite XAD-4 column
2-Florisil

TLC
Developing solvents:
1-CHCl3:
methanol 93:7
2-Toluene:
acetone:
methanol
5:3:2

DON

20–50/NA

1000

93

 

 

T-2

100–500/

2000

83

 

 

NA

 

 

 

 

HT-2

100–500/

2000

92

 

 

NA

 

 

 

 

NIV

20–50/NA

1000

82

 

 

FX

20–50/NA

1000

90

 

 

ZEN

10–50/NA

2000

88

 

 

DAS

100–500/

2000

102

 

 

NA

 

 

 

 

NEO

100–500/

2000

108

 

 

NA

 

 

 

 

Butenolide

100–500/

2000

92

 

 

NA

 

 

 

 

Moniliform

200–500/

2000

76

 

 

NA

 

 

 

 

Kim et al. (1993) modified from Tanaka, 1985)

Barley, maize

40

CH3CN:H2O
3:1, 160 ml
30 min

Hexane
Florisil column

GC–MS
TMS
derivatives

DON

5

200

92–105 (barley)

 

 

3-AcDON

5

 

87–95 (maize)

 

 

15-AcDON

5

 

 

 

 

NIV

5

 

 

 

 

4-ANIV

5

 

 

 

 

Langseth (2000a,b)

Cereals

25

CH3CN:H2O
84:16,
homogenize

Mycosep 225

GC–MS
PFPA
derivatives

DON

20–30

400

90

 

 

3-AcDON

 

 

 

 

 

NIV

 

400

72

 

 

FX

 

 

 

 

 

T-2

30

400

90

 

 

HT-2

20

400

91

 

 

Scirpentriol

 

 

 

 

 

MAS

 

 

 

 

 

DAS

 

 

 

 

 

Langseth & Claasen (1992)

Cereals

25

CH3CN:H2O
84:16,
homogenize

Charcoal/ celite/ alumina column

GC–ECD
TMS
derivatives

DON

10/30

400

80–110

 

 

3-AcDON

 

400

 

 

 

NIV

 

400

 

 

 

FX

 

400

 

 

 

Langseth & Elen (1996)

Cereals

25

CH3CN:H2O
84:16,
homogenize

Charcoal/ celite/ alumina column, hexane, silica cartridge

GC–ECD
TMS
derivatives

 

 

 

 

 

 

Lauren & Agnew (1991)

Grains

20

CH3CN:CH3OH:
H2O, 80:5:15
100 ml, 2 h

Alumina–carbon cation exchange resin, hydrolysis

HPLC C-8
GC–ECD
TFAA
derivatives

DON

10*

 

 

 

 

Lew et al. (2000)

Maize

25

CH3CN:H2O
84:16, 100 mL
shake 80 min

Mycosep No.
227 column

GC–ECD
Type B, TMS
derivatives
Type A, HFBI
derivatives

DON

50

 

 

 

 

NIV

50

 

 

 

 

3-AcDON

50

 

 

 

 

15-AcDON

50

 

 

 

 

Luo et al. (1990)

Maize, wheat

40

CH3CN:H2O
3:1, 160 ml
shake 30 min

Hexane
Florisil column

GC–MS
TMS
derivatives

DON

5

 

97–103

 

 

NIV

5

 

97–104

 

 

T-2

100

 

97–105

 

 

15-AcDON

100

 

97–106

 

 

HT-2

100

 

97–107

 

 

Mallman (2000)

Cereals

50

CH3CN:H2O
84:16, 100 mL

Mycosep No.
224, automatic

HPLC C-18

DON

100

 

 

 

 

Marasas
et al.
(1979)

Maize

50

Hexane, 100 mL
methanol:1%
KCl , 55:45
200 mL

Hexane
chloroform

GC–MS
TMS
derivatives

DON

100/NA

 

60

 

 

DAS

100/NA

 

90

 

 

T-2

100/NA

 

87

 

 

Marx et al. (1995)

 

20

CH3CN:H2O
3:1, 200 mL

Hexane
Florisil
Sep-pak

HPTLC

DON

50

 

 

 

 

Möller & Gustavsson (1992)

Cereals

50

Ethyl acetate:
acetonitrile 4:1
250 ml + 10 ml
water, shake
30 min

Hexane
Sep Pak Florisil cartridge

GC–ECD
TMS
derivatives

DON

 

250

89

 

 

FX

 

250

87

 

 

NIV

 

250

72

 

 

3-AcDON

 

250

93

 

 

DAS

 

250

89

 

 

Tricho- thecins

 

250

115

 

 

NEO

 

250

97

 

 

HT-2

 

250

94

 

 

T-2

 

250

84

 

 

Möller & Gustavsson (1992)

Cereals

50

Ethyl acetate:
acetonitrile 4:1
250 ml + 10 ml
water, shake 30 min

Hexane
Sep Pak Florisil
cartridge

GC–ECD
TMS
derivatives

DON

 

250

86

 

 

FX

 

250

84

 

 

NIV

 

250

68

 

 

3-AcDON

 

250

89

 

 

DAS

 

250

105

 

 

Tricho- thecenes

 

250

81

 

 

NEO

 

250

93

 

 

HT-2

 

250

77

 

 

T-2

 

250

79

 

 

Neira et al. (1997)

Wheat products

Pacin et al. (1997)

Pacin et al. (1997)

Pacin et al. (1997)

GC–ECD HFB
derivatives

DON

6/17

 

 

 

 

Niessen et al. (1993)

Beer

20 ml

 

 

ELISA

DON

50 ng/ml

50

45

 

 

500

77

 

 

1000

83

 

 

Pacin et al. (1997)
(modified Romer® MY 8402s)

Wheat products
(with fat)

25

1-n-hexane, 2-acetonitrile:H2O
84:16, 100 mL
blend 3 min

Mycosep No. 225

TLC

DON

25/48

100

102

 

 

250

87

 

 

500

92.4

 

 

 

 

 

 

Park et
al. (1992)

Barley

Luo et al.
(1990)

Luo et al.
(1990)

Florisil silica
cartridge

GC–ECD
TMS derivatives

DON

2

 

88–90

 

 

NIV

 

 

 

 

 

Pettersson (1993)

Barley, oats, wheat

20

CH3CN:H2O
84:16

Charcoal/ alumina column

GC–ECD
TMS
derivatives

DON

10

 

 

 

 

NIV

 

 

 

 

 

T-2

20–50

 

 

 

 

HT-2

10/30

 

 

 

 

DAS

 

 

 

 

 

3-AcDON

 

 

 

 

 

Romer Labs Inc. (1994); Lops et al. (1998)

Wheat

25

CH3CN:H2O
84:16, 100 ml
blend 3 min

Mycosep No. 224

TLC, tolueno:
ethyl acetate:
formic acetate
5:4:1

DON

500/NA

 

> 85

 

 

Ryu et al. (1996)

Barley, maize

20

CH3CN:H2O
3:1, 200 ml
shake 30 min

Hexane
Florisil column

GC–MS
TMS
derivatives

DON

5

 

83.8

 

 

T-2

5

 

88.2

 

 

HT-2

5

 

91.3

 

 

NIV

5

 

91.8

 

 

FX

5

 

90.9

 

 

3-AcDON

5

 

87.9

 

 

Schollenberger et al. (1998)

Cereals, cereal foods

10

Tanaka et al. (1985)

Hexane
Florisil cation
exchange
cartridge

GC–MS
TFAA
derivatives

DON

7/23

50–500

83–98

 

 

T-2

2/6

50–500

87–110

 

 

HT-2

5/18

50–500

74–109

 

 

NIV

12/38

50–500

71–107

 

 

FUS

6/21

50–500

82–120

 

 

15-AcDON

7/22

50–500

73–108

 

 

3-AcDON

5/16

50–500

88–110

 

 

DAS

7/22

50–500

82–116

 

 

Schwadorf & Müller
(1991)

Barley, oats, wheat

20

Tanaka et al. (1985)

Tanaka et al. (1985)

GC–MS
TFA
derivatives

NIV

15

 

84.7

 

 

DON

15

 

89.1

 

 

3Ac-DON

15

 

81.3

 

 

FX

15

 

 

 

 

HT-2

15

 

79.6

 

 

T-2

15

 

80.2

 

 

DAS

15

 

77.8

 

 

15-AcDON

15

 

83.2

 

 

Scott et
al. (1981)

Cereals

50

Methanol:
H2O
1+1, 250 mL

Partition: aqueous ammonium
sulfate 30%/
ethyl acetate,
silica gel column

GC–ECD
HFBI
derivatives

DON

10

100 (wheat

72, 73,

 

 

flour)

86, 70

 

 

1000 (wheat

85, 59,

 

 

flour)

78, 68

 

 

100 (wheat)

101, 102

 

 

500 (wheat)

77, 88

 

 

1000 (wheat)

78, 86

 

 

Scott et al. (1986)

Cereals

50

Methanol:
H2O
7:3, 150 ml

Partition: aqueous ammonium
sulfate 30%/
ethyl acetate,
silica gel column

GC–ECD
TMS
derivatives

DON

150/NA

 

 

 

 

NIV

 

 

 

 

 

Scott et al. (1989)

Cereals

50

Methanol:
H2O
7:3, 150 mL

Partition: aqueous ammonium
sulfate 30%/
ethyl acetate,
silica gel column

GC–ECD
TMS
derivatives:
DON and NIV
HFB derivatives: other trich-othecenes

DON

20/50

800 (wheat)

81

 

 

NIV

200

 

 

 

 

T-2

200/400

4000 (wheat)

86

 

 

HT-2

50/200

2000 (wheat)

82

 

 

DAS

200

 

 

 

 

Scott et al.
(1993)

Beer

10

Chem Elut CE
1020, Varian

C-18 SPE
(Supel-clean, ) Supelco

GC–MS
HFB
derivatives

DON

0.1–1.5

5–20 ng/ml

103

 

 

NIV

0.01–0.3

 

 

 

 

Solovey et al. (1999) (modified Romer® products
MY 8402s)

Maize, wheat. maize and wheat

25

CH3CN:H2O
84:16, 100 mL
blend 3 min

Mycosep No. 225

TLC

DON

25/48

100

82

 

 

 

 

 

300

86

 

 

Spanjer (2000)

Cereals, cereal products

25

PEG:H2O
5 g/400 ml

immunoaffinity column DON testTM HPLC
(VICAM)

HPLC–UV
RP18

DON

16/32

146–1070

92–103

13

 

Stratton et al. (1993)

Wheat, barley

50

Acetonitrile:H2O
21:4, 250 ml
shake 2 h

n-Hexane
LC–NH2 solid
phase extraction column

HPLC C-18
column
UV

T-2

150/NA

400 (wheat)

84.7

 

 

DON

50/NA

100 (wheat)

89.8

 

 

HT-2

120/NA

400 (wheat)

84.9

 

 

DAS

70/NA

 

 

 

 

Charcoal/celite/ alumina column

DON, 220 nm
T-2, HT-2, 200 nm, mobile phase, methanol: H2O

 

 

 

 

 

 

Sydenham & Thiel (1987)

Maize, oats

50

Methanol: water
1:1, shake 30 min

Extrelut 20 column
Silica gel cartridge

GC–ECD
HFBI
derivatives

T-2

100/NA

 

88.0

5

 

DAS

100/NA

 

88.2

4.4

 

Tanaka et
al. (1985)

cereal

20

CH3CN:H2O
3:1, 200 ml shake 30 min

Hexane
Florisil
Sep-pak

GC–ECD
TMS derivatives

DON

2/NA

300

87

 

 

NIV

2/NA

300

86

 

 

Trucksess et al. (1984); Eppley et al. (1986)

Wheat, maize

50

CH3CN:H2O
84:16, 200 mL

Charcoal/ celite/ alumina column

TLC
chloroform:
acetone:
2-propanol 8:1:1

DON

50/NA

77–93

50 ppb,
45

87

300 ppb,
39

40

1000 ppb,
64

64

Trucksess et al. (1987)

Wheat

50

Acetonitrile:
H2O: methanol
70:25:5, 200 mL
shake 60 min

Lead acetate
Charcoal/ celite/ alumina column
Octa-decylsilane
column

HPTLC
1-chloroform:
acetone:
2-propanol 8:1:1
2-chloroform:
acetone:2- propanol 7:1.5:1.5

DON

50

50

61.3

 

 

 

 

100

85

 

 

 

 

200

81.5

 

 

NIV

 

 

 

 

 

FX

 

 

 

 

 

Trucksess et al. (1996)

White flour

25

CH3CN:H2O
84:16, 100 mL
blend 3 min or shake 30 min

Mycosep No.
225 column

HPLC
Novapack C18
column

DON

20/500

500

95

7.52

11.46

1000

84

5.72

18.98

2000

85

3.14

12.72

Tutelyan et al. (1990)

Wheat

25

CH3CN:H2O
84:16, 125 mL

Charcoal/ alumina column

HPLC, silica gel column, UV (224 nm) mobile phase, hexane:isopro- panol: H2O 75:25:1.5

DON

50/NA

500

90

 

 

Vega et al. (1994) (Romer method®)

Wheat

25

CH3CN:H2O
84:16, 100 mL
blend 3 min

Mycosep No. 227

HPTLC
tolueno:ethyl
acetate: formyl acetate 6:3:1

DON

10

 

 

 

 

DAS

 

 

 

 

 

HT-2

 

 

 

 

 

T-2

 

 

 

 

 

Veratox® (1998); Trucksess et al. (1995)

Wheat, barley

50

H2O, 250 ml
blend 2 min

 

ELISA
(Veratox method)

DON

300/500

1000

65

 

 

2000

70

 

 

4000

78

 

 

1000

40

 

 

2000

70

 

 

4000

68

 

 

Vicam ® (1996); Lops et al. (1998)

Wheat

25

Polyethy-lene-glycol 5 g/400
mL H2O

Immuno-affinity column, DON
testTM HPLC
(VICAM)

HPLC
Supelcosil
LC-18 DAD
220 nm acetonitrile: H2O 10:90

DON

50

500

75

 

 

1000

84

 

 

2000

85

 

 

Vrabcheva et al. (1996)

Wheat

2

CH3CN:H2O
84:16, 10 mL
stir 120 min

 

ELISA
(Ridascreen
DON method) acetylate toxin before assay

DON

50

 

70–110

 

 

2

Methanol:
H2O
70:30, 8 mL, stir 60 min
CH3OH: PBS
70:30, stir 30 min

 

 

3-AcDON

 

 

 

 

 

15-AcDON

 

 

 

 

 

T-2

>40

 

 

 

 

DAS

 

 

 

 

 

Weingärtner et al. (1997)

Wheat

25

CH3CN:H2O
84:16, 100 mL
shake 90 min

Mycosep No.
225 column
derivatives

GC–ECD
TMS

DON

36/124

DON 100

 

98

3.95

NIV

33/144

DON 1000

 

80

 

3-AcDON

41/123

DON 2000

 

81

 

15-AcDON

35/124

 

 

 

 

FX

35/117

 

 

 

 

Yang et al. (1992)

Cereals, cereal products

20

H2O, 8 ml Chloroform + ethanol (8 + 2) 100 ml

Charcoal/ alumina column

ELISA

T-2

 

 

 

 

 

* Limit of detection

a For definitions of abbreviations, see end of Trichothecenes Appendix 6.

b For references, see monographs on deoynivalenol and T-2 and HT-2 toxins

 

Trichothecenes Appendix 6.

Sampling methods used in surveys summarized in Appendix A of the monograph on
deoxynivalenol and Appendices A and B of the monograph on T-2 and HT-2 toxins

Referencea

Grain

No. of samples

Site of collection

Lot size

Method of collection

Apro et al. (1987)

All

Proportional to total production of each area

 

 

Portions ­ 50 g
Automatic sampling

Eskola (2000a,b)

Cereals

 

Mills and malt houses

4–1000 t

Industry: Automatic sampling equipment: 100–200 g every 50–1000 kg

 

 

 

 

Farmers: Grain handling equipment. Several subsamples

Fonseca (1991)

Peanuts, maize, rice, beans

Proportional to size of lot

Bags or in bulk

20 t

Minimun no. of bags or points (bulk) to be sampled is a function (square root) of the lot size, portions of 200 g

Langseth & Elen (1997)

Barley, oats, wheat

Proportional to production and level of Fusarium infection

Grain loads, silos

 

Grain loads and

Olavarría (1992)

Maize, wheat, rice

Proportional to total production of each area

Harvest

8–12 t
truck

Grain handling equipment
(metal probe, 130 cm);
12–15 portions ­ 300 g

Quiroga et al. (1995)

Wheat

Proportional to total production of each area

Harvest

max 2000 ha

Portions ­ 50 g
Automatic sampling or grain-handling equipment

Resnik & Pacin (2000)

Wheat, maize

Proportional to total production of each area

Harvest

max 2000 ha

Portions ­ 50 g
Automatic sampling or grain-handling equipment

Spanjer (2000)

Wheat, rye, buck-wheat, maize, rice, oats, millet, barley, grain products

Imported and domestic

Mills, silos, retail shops

 

Automatic and hand sampling

Referencea

Grain

Sample size (kg)

Sample

Combined first sub- sample

Combined second sub- sample

Laboratory sample

Analysed sample

Apro et al. (1987)

All

Small grains (wheat, sorghum, oat, maize) = 10; peanut, soya bean, sunflower=50; cotton = 60

3 (wheat)
5 (maize)

1 (wheat)
2 (maize)

0.2

0.025

Eskola (2000a,b)

Cereals

3–100

 

 

0.5–1

 

 

0.5–1

 

 

 

 

Fonseca (1991)

Peanuts, maize, rice, beans

Homogenized and quartered into 4-kg samples

 

 

 

 

Langseth & Elen (1997)

Barley, oats, wheat

 

 

 

0.3–0.8

0.025

Olavarría (1992)

Maize, wheat, rice

5–6

 

 

 

0.025

Quiroga et al. (1995)

Wheat

10
Homogenized and quartered

3
14-mesh sieve

1
20-mesh sieve

0.2

0.025

Resnik & Pacin (2000)

Wheat, maize

10
Homogenized and quartered

3 (wheat)
5 (maize)
14-mesh sieve
Romer mill

 

 

0.05

Spanjer (2000)

Wheat, rye, buck-wheat, maize, rice, oats, millet, barley, grain products

3–5 kg for grains

Slurry prepared with water in ratio 2:3

 

0.0625 of slurry

0.025

Abbreviations for Trichothecenes Appendixes 1–6: AcDON, acetylated deoxynivalenol; 4-ANIV, 4-acetylnivalenol; APCI, atmospheric pressure chemical ionization; CBA, carboxylic acid; CD, competitive direct; DAD, diode array detection; DAS, diacetoxyscirpenol; DMAP, 4-dimethylaminopyridine; DON, deoxynivalenol; ECD, electron capture detection; ELISA, enzyme-linked immonosorbent assay; FID, flame ionization detection; FLD, fluorimetric detection; FX, fusarenon X; GC, gas chromatography; GPC, gel permeation chromatography; HFB, heptafluorobutanoyl; HFBA, heptafluorobutyric anhydride; HPLC, high-performance liquid chromatography; HPTLC, high-performance thin-layer chromatography; ic, intracerebrally; Ig, immunoglobulin; LC, liquid chromatography; LOD, limit of detection; LOQ, limit of quanitification; MAS, monoacetoxyscirpenol; MS, mass spectroscopy; NEO, neosolaniol; NIV, nivalenol; NA, not available; PEG, polyethylene glycol; RSDr, relative standard deviation for repeatability; RSDR, relative standard deviation for reproducibility; SFC, supercritical fluid chromatography; SFE, supercritical fluid extraction; SPE, solid-phase extraction; TBT, tributyl tin; TCMS, trichloromethylsilane; TFA, trifluoroacetic acid; TFAA, trifluoroacetic anhydride; TLC, thin-layer chromatography; TMA, trimethylaluminium; TMCS, trimethylchlorosilane; TMI, trimethylindium; TMS, trimethylsilyl; TMSI, trimethylsilylimidazole; UV, ultra-violet radiation; ZEN, zearalenone

a For references, see monographs on deoynivalenol and T-2 and HT-2 toxins



    See Also:
       Toxicological Abbreviations