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

FENG Shun-qing; LIANG Shu-qi; LIU Hong-tao

doi:10.12452/j.fxcsxb.241009444

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

Experimental Techniques and Methods | 更新时间：2025-02-12

- Determination of N-methylpiperazine Residue in Sildenafil Citrate by Ion Chromatography-Mass Spectrometry
- Journal of Instrumental Analysis Vol. 44, Issue 2, Pages: 364-368(2025)
- 作者机构：
  
  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
- 作者简介：
- 基金信息：
- DOI：10.12452/j.fxcsxb.241009444
  CLC： O657.63;TQ460.72
- Published：15 February 2025，
  
  Received：09 October 2024，
  
  Revised：07 November 2024，
  
  Accepted：2024-12-05
- 稿件说明：
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冯顺卿,梁淑琦,刘洪涛.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[J].分析测试学报,2025,44(02):364-368.

FENG Shun-qing,LIANG Shu-qi,LIU Hong-tao.Determination of N-methylpiperazine Residue in Sildenafil Citrate by Ion Chromatography-Mass Spectrometry[J].Journal of Instrumental Analysis,2025,44(02):364-368.
冯顺卿,梁淑琦,刘洪涛.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[J].分析测试学报,2025,44(02):364-368. DOI： 10.12452/j.fxcsxb.241009444.

FENG Shun-qing,LIANG Shu-qi,LIU Hong-tao.Determination of N-methylpiperazine Residue in Sildenafil Citrate by Ion Chromatography-Mass Spectrometry[J].Journal of Instrumental Analysis,2025,44(02):364-368. DOI： 10.12452/j.fxcsxb.241009444.

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1.0~100 μg/L范围内与峰面积呈良好线性关系，相关系数（

）为0.999 4。方法检出限为0.30 μg/g，定量下限为1.0 μg/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。

Abstract

An ion chromatography-mass spectrometry（IC-MS） method for the determination of N-methylpiperazine residue in sildenafil citrate（SC） active pharmaceutical ingredient（API） was developed. 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 concentration of N-methylpiperazine within the range of 1.0-100 μg/L was found with a correlation coefficient（

） of 0.999 4. The limit of detection of the method（MLOD） and limit of quantitation of the method（MLOQ） for N-methylpiperazine were 0.30 μg/g and 1.0 μg/g，respectively. The average recoveries at spiked levels of 0.020，0.10，0.20，0.50 μg ranged from 88.6% to 103%，with relative standard deviations（RSDs，

=3） of 0.62%-4.9%. The establish

ed 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

Keywords

ion chromatography-mass spectrometry（IC-MS）sildenafil citrateN-methylpiperazineresidue

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