The technique of determining the residues of epoetin, abamectin, doramectin and ivermectin in liver or muscle by SPE-HPLC-MS/MS is gradually maturing. Source: Food Safety Monitoring Technology (Chemical Industry Press)

Operation method

SPE-HPLC-MS/MS method

Materials and Instruments

Beef liver Beef muscle
Acetonitrile Hexane Nitrogen Triethylamine
Centrifugation C8SPE columns Cartridge filter membranes Chromatographic columns

Move

1. Extraction and purification

Weigh 2.5 g of homogenized bovine liver or muscle in a 50 mL centrifuge tube, add 8 mL of acetonitrile, moisten for 0.5 min, centrifuge at 2500 r/min for 5 min, and take the supernatant. The residual tissue was extracted once with 8 mL acetonitrile, and the supernatants of the two times were combined in a 500 mL centrifuge tube, added with 30 mL of purified water-triethylamine (30 + 0.045), passed through a C8SPE column (500 mg, 3 mL), drenched with 20 mL of acetonitrile-water-triethylamine (40 + 60 + 0.1), and blown dry; then drenched with 3 mL of n-hexane, and blown dry; eluted with 2 mL of acetonitrile The sample was collected. 4 mL of pure water and 6 uL of triethylamine were added to the acetonitrile eluate. After passing through a C8SPE column (500 mg, 10 mL), elution with 10 mL acetonitrile-water-triethylamine (30 + 70 + 0.1), blow-dry, and then elution with 8 mL n-hexane, blow-dry; finally elution with 2 mL acetonitrile, blow-dry, and collect the eluent in a 5 mL graduated tube, blow-dry with nitrogen gas at 50 ℃, and then fixed with 0.5 mL acetonitrile, and then passed through 0.45 um syringe filtration membrane into the HPLC-MS/MS analysis. MS/MS analysis.

2. Liquid-mass spectrometry tandem conditions

Chromatograph: Waters 2690;

Mobile phase: acetonitrile-water-formic acid (95 + 5 + 0.1);

Flow rate: 0.2 mL/min;

Chromatographic column: C18 column, 150 mm, 2.1 mm, 3 um; column temperature: (20 ± 2)℃;

Injection volume: 1O0L;

Mass spectrometer: electrospray ionization (ESI);

Capillary voltage: 3.2 kV;

Cone bore voltage: 70 V;

Source temperature: 120 °C ;

Atomizing gas: 300 ℃ ;

Doubling voltage: 650 V;

Collision gas: argon.

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