亲水作用色谱-质谱联用测定盐酸甲砜霉素甘氨酸酯中游离甘氨酸

HPLC-MS determination of glycine in thiamphenicol glycinate hydrochloride

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 high performance liquid chromatography -mass spec- trometry method （ HILIC - ESI/MS ） for the determination of glycine in thiamphenicol glycinate hydrochloride （TGH）. Methods： Alanine was used as the internal standard for MS quantification ; Chromatographic separation was performed on a Waters Atlantic Hilic （ 150 mm× 4.6 mm ,5 μm） column by using water （ containing 0. 1% formic acid） - acetonitrile （ containing 0. 1% formic acid） （25： 75 ） as the mobile phase ; The mass spectrometry was op- erated in positive ion mode, selective ion monitors were set at m/z 66 for glyeine and m/z 90 for alanine. Results： The standard curve was linear over the range of 0. 05 - 6 μg ·mL^- 1 （ r = 0. 9998 ） with detection limit at 0.2 ng · mL^-1 and quantification limit at 0.5 ng· mL^-1 ;The recoveries for the three spiked level （10% , 100% and 120% ） were 108.5% , 105.3% , and 99.2%, respectively. Conclusion： The established method is simple and suitable for glycine determination in TGH.