| 摘要: |
| 目的:建立健康产品(食品、保健品、药品)中非法添加利巴韦林的快速筛查及确证方法。方法:采用分散固相萃取鄄高效液相色谱(HPLC)快速筛查抗病毒药品。样品(胶囊、冲剂、片剂、口服液均可) 提取后, 加入固相萃取填料净化, 采用Phenomenex强阳离子氢型交换色谱柱(300 mm×7.8 mm),以水(稀硫酸调至pH 2.5±0.1)为流动相,流速0.5 mL/min,柱温60 ℃,检测波长207 nm。阳性样品采用液相色谱鄄串联质谱(LC﹣MS/MS)进行确证。结果:利巴韦林在0.01~0.30 mg/mL浓度范围内线性关系良好(r=0.999 7),加样回收率为100.9%,RSD为0.8%。结论:该方法可以简便、准确、灵敏地测定健康产品中非法添加的利巴韦林。 |
| 关键词: 利巴韦林 分散固相萃取 高效液相色谱 质谱 |
| DOI：doi:10.13407/j.cnki.jpp.1672-108X.2017.01.014 |
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| 基金项目:广东省药检系统科研项目,编号XJ201201 |
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| Ribavirin in Health Products by Dispersive Solid-Phase Extraction HPLC Screening and LC-MS/MS Verification Method |
| Luo Wei, Li Yanghua, Lin Qiufeng |
| (Dongguan Institute for Food and Drug Control, Guangdong Dongguan 523109, China) |
| Abstract: |
| Objective: To establish a rapid screening and confirmation method of ribavirin in antivirus health products。 Methods: The samples were screened by dispersive solid-phase extraction HPLC, and extracted and purity with solid phase extraction purification. HPLC was used with a Phenomenex Rezex ROA. Organic Acid H+ column (300 mm×7.8 mm) using water (adjusted to pH 2.5±0.1 with sulfuric acid) as the mobile phase. The detection wavelength was 207 nm and flow rate was 0.5 mL/min. The column temperature was 60 ℃. The positive samples were verified by LC-MS/MS. Results: The ribavirin curve was linear within a range of 0.01 to 0.30 mg/mL. The average recovery was 100.9% with RSD was 0.8%. Conclusion: This method is convenient, accurate and sensitive, it could be used to the determination of ribavirin in health products. |
| Key words: ribavirin dispersive solid-phase extraction high performance liquid chromatography mass spectrometric verification |
