Advisory Committee on Health Effects of Endocrine Disruptors
The Supplement II to the Intermediary Report
1.2.3.2

contents  Detailed contents  << prev  next >>

[Preparation of sample solutions]⁵
Place 1 ml serum in a 10 ml stoppered glass test tube. Add 5 ml acetonitrile, 0.5 g sodium chloride, 1 ml n-hexane and 25μl internal standard solution (4μg/ml), and shake for 3 min. After centrifuging the solution for 5 min at 3000 rpm, separate the acetonitrile layer and distil under reduced pressure. Dissolve the residue in 2 ml purified water, and extract two times with 5 ml and 3 ml n-hexane, respectively. Charge the Florisil-PSA column with the n-hexane layer, wash with 3 ml n-hexane, and elute PAE with 10 ml 5% acetone-n-hexane. Concentrate the eluent under reduced pressure, and add n-hexane to 1 ml.

[Procedure for quantitative analysis]⁶
(i) Typical GC/MS conditions
Column: Fused silica capillary column, 0.25 mm i.d., 30 m long, film thickness 0.25μm; phenylmethylsilicone as the liquid phase⁷
Column temperature: 80℃, 3 min -> 10℃/min -> 300℃, 5 min
Carrier gas: Helium, total flow rate 50 ml/min, column flow rate 1.5 ml/min
Injection port temperature: 240℃
Injection mode: Splitless
Interface temperature: 300℃
Detection method: SIM
Monitor ions: See below.

contents  Detailed contents  << prev  next >>