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

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,5 μm),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/z90离子进行选择离子监测。 结果: 本法线性范围为0.05~6 μg·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 spectrometry 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 operated in positive ion mode,selective ion monitors were set at m/z 66 for glycine 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.

1 Grassi C,De Benedetto F.Recent clinical evidence of the efficacy and safety of thiamphenicol glycinate acetylcysteinate and thiamphenicol glycinate.J Chemother,2002,14(3):279
2 Todisco T,Eslami A,Baglioni S,et al.An open,comparative pilot study of thiamphenicol glycinate hydrochloride vs clarithromycin in the treatment of acute lower respiratory tract infections due to Chlamydia pneumoniae.J Chemother,2002,14(3):265
3 Yang B,Lu Y,Zheng J,et al.Pharmacokinetics of the prodrug thiamphenicol glycinate and its active parent compound thiamphenicol in Beagle dogs following intravenous administration.Xenobiotica,2011,41(3):226
4 Albini E,Arena E,Belluco G,et al.Activity of aerosol thiamphenicol glycinate acetylcysteinate in a mouse model of S.pyogenes pneumonia.Arzneimittelforschung,1999,49(7):631
5 DAI Hong(戴红),ZHANG Xin-shen(张新申),XIAO Kai(肖凯).Determination of glycine by low pressure ion chromatography separation and conductivity detection(电导检测低压离子色谱法分析甘氨酸).Amino Acids Biotic Resour(氨基酸和生物资源),2007,29(4):49
6 FENG Zhi-qiang(冯志强),ZHOU Xing-qi(周兴起),ZHUANG Jun-yu(庄俊钰).Study on the amino acids analysis direct system for determining the content of free-glycin in dairy drinks(氨基酸分析仪测定含乳饮料中游离甘氨酸的方法研究).Mod Food Sci Technol(现代食品科技),2005,23(7):89
7 QIU Yu(邱宇),LIU Yan-li(刘艳丽),SUN Hua(孙华),et al.Determination of three kinds of amino acid content in the gluala glycine chewable lablet with pre-column derivatization by high performance liquid chromatography(HPLC柱前衍生法测定谷丙甘氨酸咀嚼片含量).J Harbin Med Univ(哈尔滨医科大学学报),2006,40(3):260
8 JIN Ying-hua(靳颖华),ZHANG Wei-dong(张卫东),QI Ping(齐平).Determination of glycine and methionine in compound glycyrrhiz in capsules by precolumn derivatization HPLC(柱前衍生化HPLC法同时测定复方甘草酸苷胶囊中甘氨酸和蛋氨酸的含量).Pharm J Chin PLA(解放军药学学报),2009,25(2):172
9 ZHAO Zhi-hong(赵志红),ZHANG Feng-qiu(张逢秋),ZHU Hui(朱慧),et al.Determination of glycin in dairy products by pre-column derivatization HPLC(柱前衍生高效液相色谱法测定乳制品中甘氨酸的含量).China Food Addit(中国食品添加剂),2009(4):169