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目的:建立一种直接测定盐酸甲砜霉素甘氨酸酯(TGH)中游离甘氨酸的亲水作用色谱-质谱联用(HILIC-ESI/MS)方法。方法:选用丙氨酸为内标化合物;色谱柱为Waters Atlantic Hilic(150 mm×4.6 mm,5μm),以0.1%甲酸溶液-0.1%甲酸乙腈溶液(25∶75)为流动相;在电喷雾正离子模式下,对m/z 76与m/z 90离子进行选择离子监测。结果:本法线性范围为0.05～6μg.mL-1(r=0.9998);检测限与定量限分别为0.2 ng.mL-1与0.5 ng.mL-1;低、中、高3个水平加标回收率分别为108.5%,105.3%,99.2%。结论:本法操作简便,重复性好,可用于TGH中游离甘氨酸的测定。
Objective: To establish a hydrophilic interaction chromatography-mass spectrometry (HILIC-ESI / MS) method for the direct determination of free glycine in thiamphenicol hydrochloride (TGH). METHODS: Alanine was used as the internal standard. The column was Waters Atlantic Hilic (150 mm × 4.6 mm, 5 μm) with 0.1% formic acid-0.1% formic acid in acetonitrile (25:75) In positive mode, selective ion monitoring of m / z 76 and m / z 90 ions is performed. Results: The linear range of this method was 0.05-6μg.mL-1 (r = 0.9998). The limits of detection and quantification were 0.2 ng.mL-1 and 0.5 ng.mL-1, respectively. The standard recoveries were 108.5%, 105.3% and 99.2% respectively. Conclusion: This method is simple, reproducible, and can be used for the determination of free glycine in TGH.