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气相色谱-质谱联用检测及定量分析动物饲料中的林可霉素

Gas chromatographic-mass spectrometric detection and quantitation of lincomycin in animal feedingstuffs.

作者信息

McMurray C H, Blanchflower W J, Rice D A

出版信息

J Assoc Off Anal Chem. 1984 May-Jun;67(3):582-8.

PMID:6547713
Abstract

A substantially improved assay was developed for lincomycin A in animal feedingstuffs. The assay allows unambiguous quantitation of at least 0.1 ppm in feed. Lincomycin B did not interfere because of differences in both retention time and mass of the main fragment ion in electron impact (EI) spectra. The assay using single ion monitoring with EI detection would not discriminate between lincomycin A and clindamycin. The presence of the latter was easily confirmed by using gas chromatography-mass spectrometry in the chemical ionization mode. The assay for lincomycin A was linear in the range 0-40 ng applied to the gas chromatographic column. The recovery was 93.4 +/- 4.2% at 1 and 5 ppm and 86.2 +/- 5.5% at 0.1 ppm in feed. The coefficient of variation of the assay was 4.8% at both 1 and 5 ppm, and was 6.43% at 0.1 ppm.

摘要

开发了一种用于测定动物饲料中林可霉素A的显著改进的分析方法。该分析方法能够明确测定饲料中至少0.1 ppm的含量。由于林可霉素B在电子轰击(EI)光谱中的保留时间和主要碎片离子质量存在差异,因此不会产生干扰。采用EI检测的单离子监测分析方法无法区分林可霉素A和克林霉素。通过使用化学电离模式的气相色谱-质谱联用技术可以轻松确认后者的存在。林可霉素A的分析方法在应用于气相色谱柱的0-40 ng范围内呈线性。在饲料中1 ppm和5 ppm时回收率为93.4±4.2%,在0.1 ppm时为86.2±5.5%。该分析方法在1 ppm和5 ppm时的变异系数均为4.8%,在0.1 ppm时为6.43%。

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