Protocols

Experiment for the determination of residues of eprinomectin, abamectin, doramectin and ivermectin in liver or muscle

Summary

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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Categories: Protocols
Explore topics: Biochemistry Lab

Da — when not otherwise indicated, molecular weight units are daltons.   Mw — weight-average molecular weight.   Mn — number-average molecular weight.

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Cite this article

Aladdin Scientific. "Experiment for the determination of residues of eprinomectin, abamectin, doramectin and ivermectin in liver or muscle" Aladdin Knowledge Base, updated 24 dic 2024. https://www.aladdinsci.com/us_es/faqs/experiment-for-the-determination-of-resi-en.html
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