Determination of potential genotoxic impurity in ecabet sodium active pharmaceutical ingredient by HPLC-MS/MS

被引：0

作者：

Ding Xiying ^{[1
,2
]}

Ji Xiaolong ^{[3
]}

Li Bo ^{[1
,2
]}

Mao Baiyang ^{[4
]}

Yan Fang ^{[1
,2
]}

Di Bin ^{[1
,2
]}

机构：

[1] China Pharmaceut Univ, Jiangsu Key Lab Drug Design & Optimizat, Nanjing 210009, Jiangsu, Peoples R China

[2] China Pharmaceut Univ, Dept Pharmaceut Anal, Nanjing 210009, Jiangsu, Peoples R China

[3] Yabang Pharmaceut Res Inst, Dept Synth, Changzhou 213161, Peoples R China

[4] Yabang Pharmaceut Co Ltd, Changzhou 213161, Peoples R China

来源：

JOURNAL OF CHINA PHARMACEUTICAL UNIVERSITY | 2018年 / 49卷 / 03期

关键词：

Ecabet sodium; Genotoxic impurities; HPLC-MS/MS;

D O I：

10.11665/j.issn.1000-5048.20180310

中图分类号：

R9 [药学];

学科分类号：

1007 ;

摘要：

To develop a sensitive analytical method for the determination of the genotoxic impurity mono ethyl ester of ecabet (Imp-I) , an HPLC-MS/MS technique was employed. Imp-I was synthesized according to the previous literatures. MS/MS and NMR were used to confirm the structure of Imp-I. A Thermo C-18 column was used for chromatographic separations. The mobile phase consisting of A:5 mmol/L ammonium acetate (pH adjusted to 3. 0 with formic acid) and B: acetonitrile, with a gradient program: 0 min 50% B, 4 min 50% B, 12 min 80% B, 16 min 80% B, 16. 1 min 50% B and 20 min 50% B. The column was maintained at 40 degrees C throughout the analysis. All measurements were carried out with the mass spectrometer operated under the negative ESI mode. The selective reaction monitor (SRM) transition was used. Good linearity was obtained for Imp-I over the concentration range of 4-150 ng/mL with the coefficient of determination (r) of 0. 999. And the LOQ was 4 ng/mL. A rapid and sensitive HPLC-ESI-MS/MS method was developed for quantitative analysis of Imp-I in ecabet sodium APIs. This method can be of used for quality assurance of ecabet sodium in bulk commercial drugs.

引用

页码：317 / 321

页数：5

共 16 条

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