Determination of pirlimycin residue in milk by liquid chromatographic analysis of the 9-fluorenylmethyl chloroformate derivative.

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Heller DN

Determination of pirlimycin residue in milk by liquid chromatographic analysis of the 9-fluorenylmethyl chloroformate derivative.

J AOAC Int. 1997 Sep-Oct;80(5):975-81.

PubMed ID
9325575 [ View in PubMed
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Abstract

A procedure to determine pirlimycin residues in bovine milk was developed. Pirlimycin was extracted from milk after protein precipitation and 2 stages of liquid-liquid partitioning. The extract was evaporated to dryness, redissolved in dilute base, and derivatized with 9-fluorenylmethyl chloroformate (Fmoc) to impart a chromophore for ultraviolet (UV) detection. The derivatized extract was analyzed by reversed-phase liquid chromatography (LC). Pirlimycin concentration was calculated from the peak height of the extract by using a linear regression standard curve prepared from a series of derivatized standards. The procedure's performance in the range of the regulatory tolerance (0.4 ppm) was validated by replicate analysis of control, fortified control, and residue-incurred bovine milk. Average recoveries at 0.2, 0.4, and 0.8 ppm were 91, 88, and 87%, respectively, and coefficients of variation were 5, 4, and 1%, respectively. Overall recovery for all samples was 89%, with 4% coefficient of variation. Linear regression analysis of LC/UV results versus results from a previously published LC/mass spectrometric assay gave a slope of 0.95, with a correlation coefficient of 0.98.

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