色谱2018，Vol.36Issue(2)：159-166,8.DOI:10.3724/SP.J.1123.2017.10014
串联双柱固相萃取-高效液相色谱-电喷雾多级质谱法测定盐酸二甲双胍制剂中的盐酸二甲双胍及残留物三聚氰胺和双氰胺
Determination of metformin hydrochloride,melamine and dicyandiamide in metformin hydrochloride preparations by tandem dual solid phase extraction cartridges-high performance liquid chromatography-electrospray ionization multi-stage mass spectrometry
摘要
Abstract
A method for the confirmation and quantification of metformin hydrochloride and its relative substances melamine and dicyandiamide using tandem dual solid phase extraction (SPE)cartridges and high performance liquid chromatography-electrospray ionization multi-stage mass spectrometry(HPLC-ESI-MSn)was developed. The samples were extracted with anhydrous ethanol containing 0.1%(v/v)acetic acid under ultrasound-assisted conditions. The extracts were concentrated and purified using Cleanert PCX and C18 tandem dual solid phase extraction cartridges,and eluted with 5%(v/v)ammonia methanol solution. The separation was performed on a Kromasil-C18 column(100 mm×4.6 mm,3.5 μm)with gradient elution. The detection was performed in selected ion monitoring(SIM)mode using electrospray ioniza-tion multi-stage mass spectrometry. The external standard method was used for quantification. The extraction solvents,types of SPE cartridges and eluents were optimized by comparing the recoveries under different conditions. The results showed that the detector response of each tar-get compound was linear in corresponding mass concentration ranges with the correlation coef-ficients(r2)≥0.999 2. The limits of detection(LODs)and the limits of quantification(LOQs) of the three analytes were 1.48-13.61 μg/kg and 5.96-45.67 μg/kg,respectively. The recov-eries of the three analytes were 65.02%-118.33% spiked at low,medium and high levels. The relative standard deviations(RSDs)were no more than 13.41%. The method is reliable,easy, and has a better purification effect. The method can be applied to the routine analysis of met-formin hydrochloride and its relative substances melamine and dicyandiamide in different prepa-rations of metformin hydrochloride.关键词
高效液相色谱-电喷雾多级质谱/串联双柱固相萃取/盐酸二甲双胍制剂/三聚氰胺/双氰胺Key words
high performance liquid chromatography-electrospray ionization multi-stage mass spectrometry(HPLC-ESI-MSn)/tandem dual solid phase extraction(SPE)cartridges/met-formin hydrochloride preparations/melamine/dicyandiamide分类
化学化工引用本文复制引用
周艳芬,王芳焕,王泽岚,詹海鹃,刘万毅,孟哲..串联双柱固相萃取-高效液相色谱-电喷雾多级质谱法测定盐酸二甲双胍制剂中的盐酸二甲双胍及残留物三聚氰胺和双氰胺[J].色谱,2018,36(2):159-166,8.基金项目
宁夏自然科学基金(NZ16036) （NZ16036）
宁夏国内一流学科建设项目(NXYLXK2017A04) （NXYLXK2017A04）
西部地区建设一流大学的重大创新项目(ZKZD2017003).Natural Science Foundation of Ningxia(No. NZ16036) （ZKZD2017003）
National First-Rate Discipline Construction Project of Ningxia(No. NXYLXK2017A04) （No. NXYLXK2017A04）
Major Innovations Project for Building First-Class Universities in China's Western Region(No. ZKZD2017003). （No. ZKZD2017003）
