Sensitivity enhancement of aminoglycosides in hydrophilic interaction liquid chromatography with tandem mass spectrometry by post-column addition of trace sodium acetate in methanol
Sensitivity enhancement of aminoglycosides in hydrophilic interaction liquid chromatography with tandem mass spectrometry by post-column addition of trace sodium acetate in methanol
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DOI：
10.1080/19440049.2017.1388543
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发表时间：
2018-01-01
影响因子：
2.9
通讯作者：
Yamano, Testuo
中科院分区：
文献类型：
--
作者：
Asakawa, Daichi;Uemura, Masako;Yamano, Testuo
开发一种灵敏和准确的分析方法，用于监测食品，环境和临床样品中的氨基糖苷类药物，是许多目的所需要的。本研究发现，在亲水作用色谱-串联质谱中加入乙酸钠的甲醇溶液（5 mg L-1，流速0.2mL min（-1））作为柱后试剂，钠化和质子化氨基糖苷类化合物的响应增强。钠化大观霉素、卡那霉素、庆大霉素、新霉素和阿米卡星的敏感性明显高于质子化分子。链霉素和双氢链霉素只形成质子化的分子，这表明这些氨基糖苷类中胍部分的优先电离。氨基糖苷类的定量限为0.19-2.5ng/mL。值得注意的是，这是第一次使用钠化分子定量氨基糖苷类。增强技术使我们能够从食品样品的清洁过程中消除浓缩步骤。我们还提出了一种快速的分析方法，残留的氨基糖苷类在牛奶和肉类样品，验证表明该方法具有良好的准确度和精密度在日本的最大残留限量的氨基糖苷类（40-500 μ g kg（-1））。该方法应用于污染的牛组织显示卡那霉素的残留水平非常高。该方法不仅适用于食品中氨基糖苷类抗生素的检测，而且适用于环境样品和人体血浆中氨基糖苷类抗生素的检测。
The development of a sensitive and accurate analytical method for monitoring aminoglycosides in food, environmental, and clinical samples is needed for many purposes. This study found that the responses of sodiated and protonated aminoglycosides in hydrophilic interaction chromatography with tandem mass spectrometry were enhanced upon addition of sodium acetate in methanol (5mg L-1 at a flow rate of 0.2mL min(-1)) as a post-column reagent. The sensitivities of sodiated spectinomycin, kanamycin, gentamicins, neomycin, and amikacin were significantly higher than those of the protonated molecules. Streptomycin and dihydrostreptomycin only formed protonated molecules, suggesting the preferential ionisation of the guanidine moieties in these aminoglycosides. The limits of quantification of these aminoglycosides were 0.19-2.5ng mL(-1). Notably, this is the first quantification of aminoglycosides that uses the sodiated molecules. The enhancement technique enables us to eliminate a concentration step from the clean-up process from food samples. We also proposed a rapid analytical method for residual aminoglycosides in milk and meat samples; validation showed good accuracy and precision of this method at the Japanese maximum residual limits of aminoglycosides (40-500 mu g kg(-1)). The application of this method to contaminated bovine tissues revealed remarkably high residual levels of kanamycin. This technique will be useful for the sensitive detection of aminoglycosides not only in food, but also in environmental samples and human plasma.