BS EN 14362-1-2012 禁用偶氮染料释放芳香胺欧盟测试方法(6)

Reagent 2:

Detection

2. UV lamp and /or after successive treatment with Reagents 1 and 2. Reaction time approximately 5 minutes.

A.2.2

Plates (TLC): Applied volume: Mobile solvent 3: Mobile solvent 4: Development:

--`,,```,,,,````-`-`,,`,,`,`,,`---

silica gel 60, (20 × 10) cm with fluorescence indicator F254; 10,0 µl, applied as a line;

chloroform/ethyl acetate/acetic acid (60 + 30 + 10) parts per volume; chloroform/methanol (95 + 5) parts per volume; n-butyl acetate/toluene (30 + 70) parts per volume; Saturated chamber.

2

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禁用偶氮染料释放芳香胺欧盟测试方法,替代原-1&-2方法。

BS EN 14362-1:2012

EN 14362-1:2012 (E)

Mobile solvents 2 and 3: successively without drying out the plates. Detection: 1. TLC plates with fluorescence indicator F254

2. UV lamp and/or after successive treatment with reagents 1 and 2, reaction time approximately 5 minutes. A.2.3

Plates (TLC): silica gel 60, (20 × 20) cm2

; Applied volume: 10,0 µl, applied as a line;

Mobile solvent 2: Chloroform/ethyl acetate/acetic acid (60 + 30+ 10) parts per volume; Mobile solvent 3: Chloroform/methanol (95 + 5) parts per volume; Mobile solvents 2 and 3: successively without drying of the plates; Development:

Saturated chamber.

A.3 High performance liquid chromatography (HPLC)

A.3.1 High performance liquid chromatography/diode array detector (HPLC/DAD)

Eluent 1: Methanol

Eluent 2:

Dissolve 0,68 g Potassium dihydrogen phosphate in 1000 ml water, subsequently add 150 ml methanol

Stationary phase: Zorbax Eclipse XDB C18 (3,5 µm); (150 × 4,6) mm Flow rate: 0,6 - 2,0 ml/min (flow gradient, see below) Column temperature: 32 °C Injection volume: 5 µl

Detection: DAD, spectrograph Quantification: at 240 nm, 280 nm, 305 nm and 380 nm Gradient: Time [min.]: Eluent 1 [%]: Flow [ml]: 0,00 10,0 0,6 22,50 55,0 0,6 27,50 100,0 0,6 28,50 100,0 0,95 28,51 100,0 2,0 29,00 100,0 2,0 29,01 10,0 2,0 31,0 10,0 0,6 35,00 10,0 0,6

A.3.2 High performance liquid chromatography/mass selective detector (HPLC/MS)

Eluent 1:

Acetonitrile;

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Eluent 2: 5 mmol ammonium acetate in 1 000 ml water, pH = 3,0; Stationary phase: Zorbax Eclipse XDB C18®

(3,5 µm); (2,1 × 50) mm;

Flow rate: 300 µl/min;

Gradient: start 10 % eluent 1, increase to 20 % eluent 1 within 1,5 min,

linear increase to 90 % eluent 1 within 6 min; Column temperature:

40 °C;

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