色谱

色谱 ›› 2015, Vol. 33 ›› Issue (4): 419-422.DOI: 10.3724/SP.J.1123.2014.11014

• 技术与应用 • 上一篇    下一篇

高效液相色谱法测定药品中的乙二醇二乙醚二胺四乙酸

罗宁, 刘平怀, 吴晓娜, 陈晨, 张玲, 何沂飞   

  1. 海南大学, 教育部热带多糖资源利用工程研究中心/热带作物种质资源保护与开发利用教育部重点实验室, 海南 海口 570228
  • 收稿日期:2014-11-12 修回日期:2015-02-03 出版日期:2015-04-08 发布日期:2015-03-30
  • 通讯作者: 刘平怀
  • 基金资助:

    国家科技支撑计划项目(2011BAD14B01);海南省中药现代化科技专项(ZY201327);国家科技型中小企业技术创新基金项目(13C26244604892).

Determination of ethylene glycol bis(2-aminoethyl) ether-N,N,N,N-tetraacetic acid in medicine using high performance liquid chromatography

LUO Ning, LIU Pinghuai, WU Xiaona, CHEN Chen, ZHANG Ling, HE Yifei   

  1. Key Study Center of the National Ministry of Education for Tropical Resources Utilization/Ministry of Education Key Laboratory of Protection, Development and Utilization of Tropical Crop Germplasm Resources, Hainan University, Haikou 570228, China
  • Received:2014-11-12 Revised:2015-02-03 Online:2015-04-08 Published:2015-03-30

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206

被引次数

1

摘要：

建立了高效液相色谱分析方法用来测定药品中乙二醇二乙醚二胺四乙酸(EGTA)含量,通过检测EGTA与Cu2+的配合物EGTA-Cu来检测EGTA。采用Ultimate-AQ C18色谱柱(250 mm×4.6 mm, 5 μm),流动相为乙腈-四丁基氢氧化铵水溶液(质量分数约0.3%四丁基氢氧化铵水溶液,醋酸调pH 6.50)-醋酸钠溶液(35 mmol/L醋酸钠,醋酸调pH 6.50)(20:20:60, v/v/v),检测波长为245 nm,流速为1.50 mL/min,柱温为40 ℃,进样量为100 μL。结果表明,EGTA质量浓度在0.10~15.00 mg/L范围内线性关系良好(R=0.9998);以信噪比(S/N)为3及10确定检出限和定量限,分别为0.05 mg/L和0.17 mg/L;样品加标平均回收率为98.34%~99.03%, RSD为1.08%~3.33%(n=9)。该方法操作简便,具有分离度好、灵敏度高、重复性好、回收率高等特点,适合药品中EGTA含量的检测,为EGTA检测提供了一种有效的检测方法。

关键词: 高效液相色谱, 药品, 乙二醇二乙醚二胺四乙酸

Abstract:

A method was developed for the determination of ethylene glycol bis(2-aminoethyl) ether-N,N,N,N-tetraacetic acid (EGTA) by high performance liquid chromatography (HPLC). The content of EGTA can be determined by that of EGTA-Cu through the complexation between EGTA and Cu2+. The chromatographic separation was performed on an Ultimate-AQ C18 analytical column (250 mm×4.6 mm, 5 μm) using the mobile phase of acetonitrile-ion-pairing reagents (with 0.3% tetrabutyl ammonium hydroxide in mass fraction adjusted to pH 6.50 using acetate)-buffered saline (35 mmol/L sodium acetate of pH 6.50) (20:20:60, v/v/v). The chromatographic conditions were as follows: flow rate, 1.50 mL/min; detection wavelength, 245 nm; injection volume, 100 μL; column temperature, 40 ℃. Under the conditions, good linear relationships between the mass concentration and the peak area of EGTA were observed in the range of 0.10-15.00 mg/L (R=0.9998). The limit of detection (LOD, S/N=3) and limit of quantitation (LOQ, S/N=10) were determined as 0.05 mg/L and 0.17 mg/L, respectively. The average recoveries were 98.34%-99.03% with the RSDs of 1.08%-3.33%(n=9). The results showed that the developed method is sensitive, accurate, reproducible and suitable for the analysis of EGTA in medicine.

Key words: ethylene glycol bis(2-aminoethyl) ether-N,N,N,N-tetraacetic acid (EGTA), high performance liquid chromatography (HPLC), medicine

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