Presep® 10% Silver Nitrate-impregnated Silica Gel
Presep® 55% Sulfuric Acid-impregnated Silica Gel

SPE Column for Halogenated Dioxins Analysis

01740_img01.jpg

Left: Presep® 10% Silver Nitrate-impregnated Silica Gel
Right: Presep® 55% Sulfuric Acid-impregnated Silica Gel

These columns are suitable for separating and evaluating halogenated dioxins.
Chlorinated dioxins are the most toxic and are internationally regulated.
Brominated dioxins are also considered to exhibit the same toxicity and properties as chlorinated dioxins, and are investigated for the effects on human health and for actual emissions from facilities.

Purpose

Presep® 10% Silver Nitrate-impregnated Silica Gel
Separation and evaluation of chlorinated and brominated dioxins

Presep® 55% Sulfuric Acid-impregnated Silica Gel1)
Purification of samples for measuring DXNs*1 / PHB*2 / polyhalogenated PAH*3(PBDE*4)

*1. DXNs: Dioxins
*2. PHB: Polyhydroxybutyrate
*3. PAH: Polycyclic aromatic hydrocarbon
*4. PBDE: Polybrominated diphenyl ether

Column Composition

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How to Use

Presep® 10% Silver Nitrate-impregnated Silica Gel

Perform the following pretreatment when using this column for the separation of chlorinated and brominated dioxins.

Conditioning
 4%(v/v) Acetone / n-Hexane 10 mL
Dry
 N2 purge*1
Heating
 105 ℃, 2 hours
Store in desiccator*2
Charge
 n-Hexane 1 mL*3
→ Containing PCDD/Fs、Co-PCBs
Elution 1
 n-Hexane 7 mL
Elution 2
 n-Hexane 2 mL
Elution 3
 4%(v/v) Acetone / n-Hexane 10 mL
→ Containing PBDD/Fs
Dry
 N2 *3
Redissolve
  • 1: N2 is recommended to pass through activated carbon.
  • 2: Please use it immediately after conditioning.
  • 3: It is recommended that the sample be pretreated with Presep® 55% Sulfate Silica Gel (Code: 293-35581).

Presep® 55% Sulfuric Acid-impregnated Silica Gel

Conditioning
 n-Hexane 20 mL
Charge
 n-Hexane 1 mL
→ Extracted according to JIS K0311, JIS0312, etc.
  Add internal standard if necessary.
Elution
 n-Hexane 19 mL
Dry
Redissolve → Add internal standard if necessary.

Application

Recovery rate of brominated and chlorinated dioxins on a 10% Silver Nitrate Silica Gel Column (n = 3)2)

Recovery rates(%)
8 mL of n-hexane 2 mL of n-hexane 10 mL of 4%acetone/n-hexane
Compounds IUPAC # Average S.D. Average S.D. Average S.D.
Native Brominated dioxins 2,3,7,8-TeBDD 96 1.8
1,2,3,7,8-PeBDD 92 3.4
1,2,3,6,7,8-HxBDD 85 4.9
1,2,3,4,6,7,8-HpBDD 96 1.9
OBDD 85 6.5
2,4,8-TriBDF 11 4.5 10 4.2 68 3.2
2,3,7,8-TeBDF* 96 1.9
2,3,4,7,8-PeBDF* 91 1.5
1,2,3,4,7,8-HxBDF* 71 1.7
1,2,3,4,6,7,8-HpBDF* 94 0.97
OBDF 85 9.5
13C-Labeled Chlorinated dioxins 2,3,7,8-TeCDD 90 25
1,2,3,7,8-PeCDD* 91 25 0.84 1.1
1,2,3,4,7,8-HxCDD 90 28 0.54 0.93
1,2,3,6,7,8-HxCDD* 80 24 0.63 0.75
1,2,3,7,8,9-HxCDD 87 24 1.1 1.3
1,2,3,4,6,7,8-HpCDD 85 24 1.5 1.9
OCDD 86 22 1.9 1.6
2,3,7,8-TeCDF* 86 25 0.65 0.15
1,2,3,7,8-PeCDF* 87 26 0.61 1.1
2,3,4,7,8-PeCDF* 65 13
1,2,3,4,7,8-HxCDF* 92 25 1 1.4
1,2,3,6,7,8-HxCDF 90 26 1.1 1.3
1,2,3,7,8,9-HxCDF 84 19 0.33 0.58
2,3,4,6,7,8-HxCDF* 83 23 0.26 0.45
1,2,3,4,6,7,8-HpCDF 84 22 0.92 1.6
1,2,3,4,7,8,9-HpCDF 93 17 1.3 2.3
OCDF 98 21 2.3 1.7
Co-PCBs 3,4,4',5-TeCB 81 88 11
3,3',4,4'-TeCB 77 92 16
3,3',4,4',5-PeCB* 126 97 18
3,3',4,4',5,5'-HxCB 169 92 18
2',3,4,4',5-PeCB 123 86 15
2,3',4,4',5-PeCB 118 90 20 0.09 0.16
2,3,3',4,4'-PeCB 105 95 22 0.06 0.1
2,3,4,4',5-PeCB 114 89 17
2,3',4,4',5,5'-HxCB 167 92 20
2,3,3',4,4',5-HxCB 156 88 21
2,3,3',4,4',5'-HxCB 157 99 15
2,3,3',4,4',5,5'-HpCB 189 102 14

*Major contributors to WHO-TEQ

Recovery rate of brominated and chlorinated dioxins in 55% Sulfuric Acid Silica Gel Column (n = 3)2)

Recovery rates(%)
20 mL of n-hexane
Compounds IUPAC # Average S.D.
Native Brominated Dioxins 2,3,7,8-TeBDD 98 2.5
1,2,3,7,8-PeBDD 97 1.9
1,2,3,6,7,8-HxBDD 90 0.86
1,2,3,4,6,7,8-HpBDD 89 3.1
OBDD 81 9.1
2,4,8-TriBDF 90 2.3
2,3,7,8-TeBDF* 94 2.7
2,3,4,7,8-PeBDF* 90 2.6
1,2,3,4,7,8-HxBDF* 89 2.3
1,2,3,4,6,7,8-HpBDF* 88 2.0
OBDF 95 2.0
13C-Labeled Chlorinated Dioxins 2,3,7,8-TeCDD 80 4.5
1,2,3,7,8-PeCDD* 95 4.8
1,2,3,4,7,8-HxCDD 93 6.3
1,2,3,6,7,8-HxCDD* 100 7.4
1,2,3,7,8,9-HxCDD 96 8.1
1,2,3,4,6,7,8-HpCDD 86 6.8
OCDD 88 8.8
2,3,7,8-TeCDF* 86 2.0
1,2,3,7,8-PeCDF* 95 6.0
2,3,4,7,8-PeCDF 66 3.8
1,2,3,4,7,8-HxCDF* 93 5.7
1,2,3,6,7,8-HxCDF 102 8.7
1,2,3,7,8,9-HxCDF 79 7.8
2,3,4,6,7,8-HxCDF* 75 8.3
1,2,3,4,6,7,8-HpCDF 82 5.2
1,2,3,4,7,8,9-HpCDF 101 5.8
OCDF 91 4.2
Co-PCBs 3,4,4',5-TeCB 81 69 2.9
3,3',4,4'-TeCB 77 74 2.1
3,3',4,4',5-PeCB* 126 79 2.9
3,3',4,4',5,5'-HxCB 169 91 6.4
2',3,4,4',5-PeCB 123 71 1.6
2,3',4,4',5-PeCB 118 70 2.4
2,3,3',4,4'-PeCB 105 77 4.4
2,3,4,4',5-PeCB 114 72 1.8
2,3',4,4',5,5'-HxCB 167 78 4.4
2,3,3',4,4',5-HxCB 156 79 3
2,3,3',4,4',5'-HxCB 157 84 6.7
2,3,3',4,4',5,5'-HpCB 189 87 5.9

*Major contributors to WHO-TEQ

  • CDD:Chlorinated Dibenzo-p-dioxin
  • CB:Chlorinated Biphenyl
  • CDF:Chlorinated Dibenzofuran
  • Di:Di-
  • Tr:Tri-
  • Te:Tetra-
  • Pe:Penta-
  • Hx:Hexa-
  • Hp:Hepta-
  • O:Octa-

References

  1. Patent No. 5691120(2015)
  2. Suzuki, G., et al.: Separate screening of brominated and chlorinated dioxins in field samples using in vitro reporter gene assays with rat and mouse hepatoma cell lines, Analytica Chimica Acta, 975, 86 (2017).

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Solvents for Dioxin analysis

Silica gel for Dioxin analysis

DIOXIN TRAP BEADS

Other dioxin analysis reagents

For research use or further manufacturing use only. Not for use in diagnostic procedures.

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