UPLC-MS/MS测定萘敏维滴眼液包材中6种抗氧剂的含量及其向药液的迁移研究  

Content of 6 antioxidants in naphazoline hydrochloride,chlorphenamine maleate and vitamin B_(12)eye drops by UPLC-MS/MS and their migration to liquid

作　　者：吴月霞 杨秋红 丰丽莼 张倩 范围 陈杰[1] WU Yue-xia;YANG Qiu-hong;FENG Li-chun;ZHANG Qian;FAN Wei;CHEN Jie(Henan Institute for Food and Drug Control,Zhengzhou 450018)

机构地区：[1]河南省食品药品检验所,郑州450018

出　　处：《中南药学》2023年第5期1347-1351,共5页Central South Pharmacy

摘　　要：目的建立超高效液相色谱串联三重四极杆质谱法(UPLC-MS/MS)考察萘敏维滴眼液包材中6种抗氧剂的含量及向药液的迁移研究。方法采用Waters ACQUITY UPLC BEH C18色谱柱(2.1 mm×50 mm,1.7μm);以0.1%甲酸水溶液为流动相A,乙腈为流动相B,进行梯度洗脱,流速为0.3 mL·min^(-1)。质谱采用电喷雾(ESI)离子源,多反应监测(MRM)正、负离子切换模式进行定性定量分析。结果6种抗氧剂均在0.5~100 ng·mL^(-1)与峰面积线性关系良好(r≥0.9997),检测限(LOD)和定量限(LOQ)分别在0.003~0.122 ng·mL^(-1)和0.010~0.432 ng·mL^(-1),平均加标回收率在98.9%~101.3%,RSD在0.23%~1.6%。经检验,25批萘敏维滴眼液中6种抗氧剂含量均不超过检测限浓度,均符合规定,包材中检出2种抗氧剂。影响因素试验表明,6种抗氧剂的迁移不受强光照射、高温和高湿的影响,表明本品由包材中抗氧剂迁移带来的安全风险较低。结论本方法操作简便、灵敏度高、准确度好、检测限低,可用于萘敏维滴眼液中6种抗氧剂迁移情况的监测、溯源及快速筛查。Obtective To establish an UPLC-MS/MS method to determine the content of 6 antioxidants in naphazoline hydrochloride,chlorphenamine maleate and vitamin B12 eye drops,and the migration of antioxidants in the package materials to the liquid.Methods Waters ACQUITY UPLC BEH C18 column(2.1 mm×50 mm,1.7μm)was used.Gradient elution was performed with 0.1%formic acid aqueous solution as mobile phase A and acetonitrile as mobile phase B at the flow rate of 0.3 mL•min^(-1).Mass spectrometry was performed with electrospray(ESI)ion source and multiple reaction monitoring(MRM)in both positive and negative ion switching modes.Results The linearity of the 6 antioxidants was good at 0.5~100 ng·mL^(-1)(r≥0.9997).The limit of detection was 0.003~0.122 ng·mL^(-1)and limit of quantification was 0.010~0.432 ng·mL^(-1).The average recoveries were 98.9%~101.3%,and RSD was 0.23%~1.6%.After the inspection,the content of 6 antioxidants in 25 batches of eye drops did not exceed the detection limit concentration,all in line with the regulations.Two antioxidants were detected in the package materials.The migration of 6 antioxidants was not affected by high light irradiation,high temperature and high humidity,indicating that the safety risk caused by the migration of antioxidants in the package materials was low.Conclusion The method is simple,sensitivte,and accurate with low detection limit,which can be used for the monitoring,tracing and rapid screening of the migration of 6 antioxidants in vitamin B12 eye drops.

关 键 词：超高效液相色谱串联三重四极杆质谱法 快速筛查 萘敏维滴眼液 抗氧剂 包材 

分 类 号：R927[医药卫生—药学]