[Analytical Method for Melengestrol Acetate in Livestock Products Using LC-MS/MS].

IF 0.2 4区 农林科学 Q4 FOOD SCIENCE & TECHNOLOGY Food Hygiene and Safety Science Pub Date : 2024-01-01 DOI:10.3358/shokueishi.65.15
Takatoshi Sakai, Hiroyuki Kikuchi, Satoru Nemoto, Hiroshi Akiyama, Takaaki Taguchi, Tomoaki Tsutsumi
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Abstract

The present study verified that it is possible to analyze melengesterol acetate using the existing multi-residue method. Melengestrol acetate was extracted from livestock products using acidic acetonitrile acidified with acetic acid in the presence of n-hexane and anhydrous sodium sulfate. The crude extracts were cleaned up using an octadecylsilanized silica gel cartridge column. Separation by HPLC was performed using an octadecylsilanized silica gel column with linear gradient elution of 0.1 vol% formic acid and acetonitrile containing 0.1 vol% formic acid. For the determination of the analyte, tandem mass spectrometry with positive ion electrospray ionization was used. In recovery tests using four livestock products fortified with maximum residue limits levels of melengestrol acetate (0.001-0.02 mg/kg), the truenesses ranged from 82% to 100%, and the repeatabilities for the entire procedure ranged from 0.5 RSD% to 5.6 RSD%. In recovery tests using 11 livestock products fortified with 0.0005 mg/kg of melengestrol acetate, the truenesses ranged from 88% to 99%, and the repeatabilities ranged from 1.3 RSD% to 5.4 RSD%. The limit of quantification for melengestrol acetate in livestock products was 0.0005 mg/kg.

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[利用 LC-MS/MS 分析畜产品中醋酸美伦孕酮的方法]。
本研究验证了使用现有的多残留法分析醋酸美伦孕酮酯是可行的。在正己烷和无水硫酸钠存在下,使用乙酸酸化的酸性乙腈从畜产品中提取醋酸美伦孕酮。粗提取物用十八烷基硅胶柱净化。使用十八烷基硅烷化硅胶柱,以 0.1 Vol% 的甲酸和含 0.1 Vol% 甲酸的乙腈线性梯度洗脱,进行高效液相色谱分离。采用正离子电喷雾串联质谱法测定分析物。在使用四种添加了醋酸美伦孕酮最高残留限量(0.001-0.02 毫克/千克)的畜产品进行的回收试验中,真实度从 82% 到 100% 不等,整个过程的重复性从 0.5 RSD% 到 5.6 RSD% 不等。在使用 11 种添加了 0.0005 毫克/千克醋酸美伦孕酮的畜产品进行的回收试验中,真实度在 88% 到 99% 之间,重复性在 1.3 RSD% 到 5.4 RSD% 之间。畜产品中醋酸美伦孕酮的定量限为 0.0005 毫克/千克。
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来源期刊
Food Hygiene and Safety Science
Food Hygiene and Safety Science Medicine-Public Health, Environmental and Occupational Health
CiteScore
0.70
自引率
0.00%
发文量
28
审稿时长
18-36 weeks
期刊介绍: Information not localized
期刊最新文献
[Analytical Method for Melengestrol Acetate in Livestock Products Using LC-MS/MS]. [Establishment of Rapid Simultaneous Analysis Method for Plant Toxins by LC-TOF-MS]. [Implementation and Evaluation of Risk Communication Regarding Residual Pesticides]. [Improved Indophenol Titration Method for Ascorbic Acid Using a Dropper and Electronic Balance: Enhanced Convenience and Efficiency]. [Comparison of DNA Extraction Methods for Processed Foods Containing Soybean or Maize].
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