摘要
目的建立检测抗鼻炎喷剂中非法添加盐酸萘甲唑林的高效液相色谱-质谱联用(LC-MS/MS)法。方法色谱柱为Zorbax Eclipse XDB-C18柱(150 mm×4.6 mm,5μm),流动相为乙腈-3%醋酸-三乙胺(15∶85∶0.08,用醋酸或三乙胺调节p H=3.0),流速0.2 m L/min,柱温35℃;电喷雾电离,正离子模式,多重反应监测扫描(MRM)方式对盐酸萘甲唑林的母离子(m/z 210)及其子离子(m/z 140,115)进行检测。结果盐酸萘甲唑林检测限低于0.05 ng。24批次市售抗鼻炎喷剂中,17批次检出盐酸萘甲唑林。结论该法专属性强、灵敏度高,可用于抗鼻炎喷剂非法添加盐酸萘甲唑林的筛选与确证工作。
Objective To develop a LC-MS/MS method for the determination of illegally added chemical substance naphazoline hy-drochloride in anti-rhinitis spray. Methods LC-MS/MS method was adopted. The separation was achieved by using the Zorbax Eclipse XDB-C18 column （ 150 mm × 4. 6 mm, 5 μm ） and the mobile phase of acetonitrile-3% acetic acid-triethylamine （ 15 ：85 ：0. 08, adjusting pH=3. 0 with acetic acid or triethylamine ） . The flow rate was 0. 2 mL/min and the column temperature was set at 35℃. The electrospray ionization was adopted. The parent ion （ m/ z 210 ） and daughter ion （ m/ z 140, 115 ） of naphazoline hydrochlo-ride were detected by the multiple-reaction monitoring scanning mode via positive ion mode. Results The limit of detection （ LOD ） for illegally added naphazoline hydrochloride in anti-rhinitis spray was below 0. 05 ng. Among the 24 batches of commercially available anti-rhinitis spray, naphazoline hydrochloride was detected out in 17 batches. Conclusion This established method is strongly specific and highly sensitive, and can be used for the screening and confirmation work of illegally added naphazoline hydrochloride in anti-rhinitis spray.
出处
《中国药业》
CAS
2015年第13期33-34,共2页
China Pharmaceuticals
基金
广东省药检系统非法添加系统技术策略专项资助课题
项目编号:YJ201074
