Determination of octylphenol, nonylphenol, bisphenol A, diethylstilbestrol, estrone, 17α-ethinyl estradiol, 17β-estradiol, and estriol residues in aquatic products-Gas chromatography-mass spectrometry (1)

1 Scope

This standard specifies the sample preparation and gas chromatography- Mass spectrometry metho.

This standard is applicable to octylphenol, nonylphenol, bisphenol A, diethylstilbestrol, estrone, 17α-ethinyl estradiol, 17β-estrone in edible tissues of aquatic products such as fish, shrimp, crab, shellfish, sea cucumber and soft-shelled turtl.

2 Normative references

The following documents are essential for the application of this documen.

GB/T6682 Analytical Laboratory Water Specifications and Test Methods

3 Principles

The residues of octylphenol, nonylphenol, bisphenol A, diethylstilbestrol, estrone, 17α-ethinyl estradiol, 17β estradiol and estriol in the sample were extracted by ethyl acetate, gel permeation chromatography and solid phase extraction Purification, derivatization with tincture of heptafluorobutyrate, determination by gas chromatography-mass spectrometry, and quantification by external standard metho.

4 Reagents and materials

Unless otherwise specified, all reagents are of analytical grade, and the water is first-grade water in accordance with GB/T6682.

1 Reagents

1 Ethyl acetate (CH3COOC2H5): chromatographically pur.

2 Acetone (CH3COCH3): chromatographically pur.

3 n-hexane (C6H14): chromatographically pur.

4 Methanol (CH3OH): chromatographically pur.

5 Cyclohexane (C6H12): chromatographically pur.

6 Heptafluorobutyric anhydride (C8F14O3.

7 Sodium carbonate (Na2CO3.

2 Solution Preparation

1 Sodium carbonate solution: Weigh 10 g of sodium carbonate, dissolve in water and dilute to 100 mL, and mix wel.

2 50% cyclohexane ethyl acetate solution: Mix equal volumes of cyclohexane and ethyl acetat.

3 50% methanol solution: Mix methanol and water in equal volum.

3 Standards

The contents of octylphenol, nonylphenol, bisphenol A, diethylstilbestrol, estrone, 17α-ethinyl estradiol, 17β estradiol, and estriol were all >90.

4 Standard solution preparation

1 Standard stock solution: take 10 mg of octylphenol, nonylphenol, bisphenol A, diethylstilbestrol, estrone, 17α-ethinyl estradiol, 17β estradiol, and estriol standard products, accurately weigh them, and place them in In a 10 mL brown volumetric flask, dissolve and dilute to the mark with methanol to prepare a standard stock solution with a concentration of 1 mg/m.

2 Mixed standard working solution: Precisely measure an appropriate amount of standard stock solution, dilute with methanol, and make up the concentration of octylphenol 50μg/L, nonylphenol, bisphenol A 30μg/L, diethylstilbestrol 50μg/L, estrone, Mixed standard working solution of 17α-ethinyl estradiol, 17β estradiol, and estriol 100 μg/.
Store at 2°C ~ 8°C away from light, valid for 1 wee.

5 Materials

1 Polystyrene gel filler: Bio-BeadsS-X3, 200-400 mes.

2 HLB solid phase extraction cartridge: 60mg/3mL, or equivalen.

3 Gel purification column: length 25cm, inner diameter 2cm, glass chromatography column with pisto.
The polystyrene gel packing soaked in 50% cyclohexane ethyl acetate solution overnight was packed into the column by wet method, and the column bed height was 20 c.
The column bed was maintained at 50% cyclohexane in ethyl acetate throughou.

5 Instruments and equipment

1 Gas chromatography mass spectrometer: equipped with EI sourc.

2 Analytical balance: Sensitivity 00001g and 01.

3 Homogenize.

4 Centrifuge: 4000r/mi.

5 Vorte.

6 Nitrogen blowe.

7 Solid phase extraction devic.

8 Polypropylene centrifuge tube: 50mL

9 Stoppered glass centrifuge tube: 10mL

10 Pear-shaped bottle: 100mL

6 Preparation and storage of samples

1 Preparation of samples

Take an appropriate amount of fresh or thawed blank or test tissue, mince, and homogenize:

a) Take the test sample after homogenization as the test material;

b) Take the homogenized blank sample as blank sample;

c) Take the homogenized blank sample, add the standard working solution of appropriate concentration, and add it as the blank sampl.

2 Storage of samples

Store below -18°.