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Single-step multiresidue determination of ten multiclass veterinary drugs in pork, milk, and eggs using liquid chromatography with tandem mass spectrometry.

Journal of separation science (2015-06-03)
Jin-A Park, Dan Zhang, Dong-Soon Kim, Seong-Kwan Kim, Kyeong-Su Cho, Dana Jeong, Jae-Han Shim, Jin-Suk Kim, A M Abd El-Aty, Ho-Chul Shin
ABSTRACT

A multiclass, multiresidue determination method is reported for the detection of ten veterinary drugs, including scopolamine, metoclopramide, acriflavine, berberine, tripelennamine, diphenhydramine, acrinol, triamcinolone, loperamide, and roxithromycin in pork, milk, and eggs. The method involves a simple extraction using 0.1% formic acid in acetonitrile, followed by defatting with n-hexane, centrifugation, and filtration prior to liquid chromatography with tandem mass spectrometric analysis. As ion suppression and enhancement effects are reported, matrix-matched calibrations are used for quantification, with determination coefficients ≥0.9765. For the majority of the tested analytes, the intra- and interday accuracy (expressed as recovery %) range from 70.6 to 94.6% and from 70.1 to 93.3%, respectively, and the precision (expressed as relative standard deviation) ranges from 0.5 to 19.8% and from 2.8 to 18.4% in all matrices. The limits of quantification range between 0.5 and 10 ng/g. The validated tandem mass spectrometry method is successfully applied to market samples; the target analytes are not detected in any of the tested samples. In terms of accuracy, no extract cleanup is deemed necessary. The developed method is feasible for the simultaneous detection of the tested analytes in pork, milk, and eggs.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Methanol, JIS 300, ≥99.8%, for residue analysis
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Methanol, ≥99.8%, for chromatography
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Methanol, ≥99.8%, suitable for absorption spectrum analysis
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Methanol, SAJ first grade, ≥99.5%
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Methanol, JIS 1000, ≥99.8%, for residue analysis
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Methanol, JIS special grade, ≥99.8%
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Acetonitrile solution, contains 0.05 % (v/v) trifluoroacetic acid
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Acetonitrile solution, contains 0.1 % (v/v) trifluoroacetic acid, suitable for HPLC
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Roxithromycin, 95.0-102.0% (HPLC)
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Triamcinolone
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Methanol, SAJ special grade
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Methanol, suitable for HPLC
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Methanol, anhydrous, 99.8%
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Acriflavine
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6,9-Diamino-2-ethoxyacridine-DL-lactate monohydrate, 99%
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Acetonitrile solution, contains 0.1 % (v/v) formic acid, suitable for HPLC
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Formic acid, ≥95%, FCC, FG
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Hexane, JIS 300, ≥96.0%, for residue analysis
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Hexane, SAJ first grade, ≥95.0%
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Formic acid, SAJ first grade, 88.0-89.5%
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Hexane, JIS 1000, ≥96.0%, for residue analysis
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Acetonitrile, ≥99.8%, for residue analysis, JIS 1000
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Formic acid, JIS special grade, ≥98.0%
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Hexane, ≥96.0%, suitable for residual phthalate analysis
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Acetonitrile, ≥99.8%, suitable for HPLC