离子色谱-质谱联用法测定枸橼酸西地那非中N-甲基哌嗪残留  

Determination of N-methylpiperazine Residue in Sildenafil Citrate by Ion Chromatography-Mass Spectrometry

作　　者：冯顺卿[1] 梁淑琦 刘洪涛[1] FENG Shun-qing;LIANG Shu-qi;LIU Hong-tao(Instrumental Analysis&Research Center of Sun Yat-sen University,Guangzhou 510275,China;School of Chemistry,Sun Yat-sen University,Guangzhou 510006,China)

机构地区：[1]中山大学分析测试中心,广东广州510275 [2]中山大学化学学院,广东广州510006

出　　处：《分析测试学报》2025年第2期364-368,共5页Journal of Instrumental Analysis

基　　金：中山大学分析测试中心实验技术方法开发及仪器改造专项(202103)。

摘　　要：建立了枸橼酸西地那非原料药中N-甲基哌嗪残留的离子色谱-质谱联用分析方法。样品中N-甲基哌嗪采用流动相超声提取,样品溶液经Cleanert IC-RP固相萃取小柱净化后,进行离子色谱-质谱分析。N-甲基哌嗪采用加热电喷雾离子源,正离子和选择离子模式下检测,外标法定量。结果表明,N-甲基哌嗪在1.0~100μg/L范围内与峰面积呈良好线性关系,相关系数(r^(2))为0.9994。方法检出限为0.30μg/g,定量下限为1.0μg/g。4个加标水平的回收率为88.6%~103%,相对标准偏差为0.62%~4.9%。该方法灵敏度高、快速准确,适用于枸橼酸西地那非原料药中N-甲基哌嗪残留的测定和确证。An ion chromatography-mass spectrometry(IC-MS)method for the determination of N-methylpiperazine residue in sildenafil citrate(SC)active pharmaceutical ingredient(API)was devel⁃oped.The N-methylpiperazine in samples was extracted by sonication with the eluent,then purified with a Cleanert IC-RP cartridge,and determined by IC-MS.The confirmation was achieved with heated electrospray ionization(HESI)in positive ion mode and selective ion monitoring(SIM)mode,and quantified by the calibration curve method.Good linear relationship between peak area and con⁃centration of N-methylpiperazine within the range of 1.0-100μg/L was found with a correlation coeffi⁃cient(r2)of 0.9994.The limit of detection of the method(MLOD)and limit of quantitation of the method(MLOQ)for N-methylpiperazine were 0.30μg/g and 1.0μg/g,respectively.The average re⁃coveries at spiked levels of 0.020,0.10,0.20,0.50μg ranged from 88.6%to 103%,with rela⁃tive standard deviations(RSDs,n=3)of 0.62%-4.9%.The established method demonstrated to be good sensitivity and high accuracy,which could be used for the determination and confirmation of N-methylpiperazine in SC API.

关 键 词：离子色谱-质谱联用(IC-MS) 枸橼酸西地那非 N-甲基哌嗪 残留 

分 类 号：O657.63[理学—分析化学] TQ460.72[理学—化学]