Simultaneous Determination of Four Estrogen Residues in Powdered Milk Using Ultrasonic Extraction-HPLC

doi:10.7506/spkx1002-6630-201412031

Abstract

Abstract:

A method was developed for the simultaneous determination of residues of ethinyl estradiol, diethylstilbestrol,
4-nonylphenol and estradiol benzoate in powdered milk by high performance liquid chromatograph (HPLC) after ultrasonic
extraction. Samples were ultrasonically extracted with acetonitrile and after centrifugation of the extract, the supernatant was
concentrated and filtrated through a 0.45 μm filter before analysis by HPLC. Extraction solvent, extraction and centrifugation
time, and HPLC conditions were optimized. The analysis was conducted by using gradient elution with acetonitrile-0.043 mol/L
NaH2PO4 buffer as the mobile phase. Under the optimized conditions, the four estrogens were separated well, and the
proposed method exhibited good reproducibility (0.95%–2.04%) and recovery (80.2%–101.0%). The calibration curves
were linear with correlation coefficient ranging from 0.992 4 to 0.999 7. The limit of detection of the method ranged from
3 to 20 μg/kg. This method proved to be rapid, sensitive and simple without interference of impurities and be able to meet
the analytical requirements for residues of these four estrogens in milk powder.

Key words: ultrasonic extraction, high performance liquid chromatography (HPLC), powdered milk, estrogen

CLC Number:

O657.72

TAN Fang, HUANG Lu, ZHENG Qi*. Simultaneous Determination of Four Estrogen Residues in Powdered Milk Using Ultrasonic Extraction-HPLC[J]. FOOD SCIENCE, doi: 10.7506/spkx1002-6630-201412031.

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Simultaneous Determination of Four Estrogen Residues in Powdered Milk Using Ultrasonic Extraction-HPLC

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