摘要
建立了同时直接测定复方氨基酸注射液(18AA)中蛋氨酸亚砜(MSO)和蛋氨酸砜(MSO2)杂质的HPLC检测方法。采用Titank C18色谱柱(4. 6 mm×250 mm,5μm),以10 mmol/L(NH4)2HPO4缓冲液(含有10 mmol/L 1-辛烷磺酸钠,用磷酸调节pH至1. 9)为流动相A,以乙腈为流动相B,进行梯度洗脱,流速1. 0 mL/min,检测波长205 nm,进样体积为100μL,柱温为4℃。结果表明,在优化条件下,蛋氨酸亚砜和蛋氨酸砜能实现有效分离。蛋氨酸亚砜和蛋氨酸砜的检测限(S/N=3)分别为0. 09μg/mL和1. 35μg/mL;定量限(S/N=10)分别为0. 31μg/mL和4. 51μg/mL;蛋氨酸亚砜、蛋氨酸砜分别在0. 31～201. 76μg/mL和4. 51～225. 72μg/mL范围内线性关系良好;加标回收率分别为99. 1%～102. 2%(蛋氨酸亚砜)和98. 2%～101. 2%(蛋氨酸砜)。该方法可在常规实验室和制药工业中对复方氨基酸注射液(18AA)中的蛋氨酸亚砜和蛋氨酸砜进行检测。
A direct and simultaneous determination of methionine sulfoxide （MSO） and methionine sulfone （MSO2） impurities in compound amino acid injection （18AA） by high performance liquid chromatography （HPLC） was developed. The determination was performed on a Titank C18 column （4.6 mm×250 mm, 5 μm） with the mobile phase consisting of acetonitrile and 10 mmol/L diammonium hydrogen phosphate buffer （containing 10 mmol/L sodium 1-octanesulfonate and obtaining pH 1.9 by addition of phosphoric acid） by gradient elution at a flow rate of 1.0 mL/min. The detection wavelength was set at 205 nm and the injection volume was 100 μL. The column temperature was set at 4 ℃. Under the optimal conditions, MSO and MSO2 were effectively separated. The limits of detection （ S/N ratio, 3 ： 1 ） and quantification （ S/N ratio, 10 ： 1 ） of MSO and MSO2 were 0.09 μg/mL and 1.35 μg/mL; 0.31 μg/mL and 4.51 μg/mL, respectively. The method was linear in the concentration ranges of 0.31 - 201.76 μg/mL for MSO and 4.51 - 225.72 μg/mL for MSO2. The relatively simple method proved accurate （recovery was 99.1% - 102.2% for MSO, 98.2% - 101.2% for MSO2 ）. The established method did not require complicated derivatization process, and was simple and accurate for the determination of MSO and MSO2 impurities in 18 AA for laboratory research and pharmaceutical industry.
作者
李莉
崔红艳
钟家棋
马炳原
李宗豪
沈梦元
顾浦中
张明
LI Li , CUI Hong-yan, ZHONG Jia-qi, MA Bing-yuan, LI Zong-hao, SHEN Meng-yuan, GU Pu- zhong , ZHANG Ming(Kangda College of Nanjing Medical University, Lianyungang 22200)
出处
《分析试验室》
CAS
CSCD
北大核心
2018年第11期1309-1314,共6页
Chinese Journal of Analysis Laboratory
基金
江苏省高等学校自然科学研究面上项目(17KJD150005)
连云港市科技计划项目(SH1627)
南京医科大学科技发展基金项目(2016NJMU011
2016NJMUZD021)
南京医科大学康达学院科研发展基金项目(KD2016GCCRCYJ01
KD2016GCCRCYJ02
KD2016KYJJZD001
KD2016KYJJZD002)资助
作者简介
通信作者:李莉,E-mail:lili@njmu.edu.cn;通信作者:张明,E-mail:mingzhang@njmu.edu.cn.
