畜产品中莫诺霉素A的LC-MS/MS分析方法[j]。

IF 0.2 4区 农林科学 Q4 FOOD SCIENCE & TECHNOLOGY
Hiroyuki Kikuchi, Takatoshi Sakai, Tomoko Okura, Satoru Nemoto, Hiroshi Akiyama, Takaaki Taguchi, Tomoaki Tsutsumi
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引用次数: 0

摘要

建立了一种简便、灵敏的畜牧产品中莫诺霉素A残留的LC-MS/MS检测方法。用氢氧化铵与甲醇(1:9,v/v)的混合物,在50℃下预热,从样品中提取黄磷脂残留定义物Moenomycin A。粗提液在氢氧化铵、甲醇和水(1:60:40,v/v/v)和乙酸乙酯的混合物中蒸发纯化。取碱性层,并用强阴离子交换(intertsep SAX)固相萃取筒清洗。色谱柱为Inertsil C8,用0.3 vol%甲酸和含有0.3 vol%甲酸的乙腈进行线性梯度洗脱。采用负离子电喷雾串联质谱法检测莫诺霉素A。回收试验使用了三种猪样本(肌肉、脂肪和肝脏)和鸡蛋。样品以0.01 mg/kg的剂量加标莫诺霉素A,并按每种样品的日本最大残留限量(MRLs)加标。准确度为0.5 ~ 2.8%,准确度为79% ~ 93%。该方法的定量限(S/N≥10)为0.01 mg/kg。该方法可用于畜产品中黄磷脂的监管监测。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
[An LC-MS/MS Analytical Method for Moenomycin A in Livestock Products].

A simple and sensitive method for the determination of moenomycin A residues in livestock products using LC-MS/MS was developed. Moenomycin A, a residual definition of flavophospholipol, was extracted from samples with a mixture of ammonium hydroxide and methanol (1 : 9, v/v) preheated at 50℃. The crude extracted solutions were evaporated and purified by liquid-liquid partitioning between a mixture of ammonium hydroxide, methanol and water (1 : 60 : 40, v/v/v) and ethyl acetate. The alkaline layer was taken, and cleaned up using a strong anion exchange (InertSep SAX) solid phase extraction cartridge. The LC separation was performed on an Inertsil C8 column with liner gradient elution using 0.3 vol% formic acid and acetonitrile containing 0.3 vol% formic acid. Moenomycin A was detected using tandem mass spectrometry with negative ion electrospray ionization. Recovery tests were conducted using three porcine samples (muscle, fat and liver) and chicken eggs. Samples were spiked with moenomycin A at 0.01 mg/kg and at the Japanese Maximum Residue Limits (MRLs) established for each sample. The trueness ranged from 79 to 93% and precision ranged from 0.5 to 2.8%. The limit of quantification (S/N≥10) of the developed method is 0.01 mg/kg. The developed method would thus be very useful for regulatory monitoring of flavophospholipol in livestock products.

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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
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