医疗装备2024,Vol.37Issue(5) :39-43.DOI:10.3969/j.issn.1002-2376.2024.05.011

超高效液相色谱-串联质谱法快速定性和定量筛查贴敷类医疗器械产品非法添加的水杨酸甲酯

Rapid Screening and Quantitative Analys of Methyl Salicylate which was Illegally Added Into the Medical Dressings by UPLC-MS/MS

刘路 皮璟渔 余永红 刘小辉 胡红刚 梁国东
医疗装备2024,Vol.37Issue(5) :39-43.DOI:10.3969/j.issn.1002-2376.2024.05.011

超高效液相色谱-串联质谱法快速定性和定量筛查贴敷类医疗器械产品非法添加的水杨酸甲酯

Rapid Screening and Quantitative Analys of Methyl Salicylate which was Illegally Added Into the Medical Dressings by UPLC-MS/MS

刘路 1皮璟渔 1余永红 1刘小辉 1胡红刚 1梁国东1
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作者信息

  • 1. 江西省医疗器械检测中心(江西南昌 330000)
  • 折叠

摘要

目的 通过建立一种利用超高效液相色谱-串联质谱法(UPLC-MS/MS),对贴敷类医疗器械非法添加的水杨酸甲酯进行定性、定量分析.方法 样品经甲醇提取、过滤后上机,采用超高效液相色谱-串联质谱法,WATERS ACQUITY UPLC BEH C18 色谱柱(2.1 mm×100 mm,1.7 μm)分离,以0.05%氨水-甲醇为流动相,进行梯度洗脱;电喷雾电离(ESI),负离子扫描,多反应监测(MRM)模式采集数据.结果 水杨酸甲酯1~100 μg/ml范围内线性关系良好,相关系数为0.9997;3 个添加水平平均加样回收率为90.3%~100.7%;相对标准偏差(RSD)为0.5%~0.9%;方法 检出限为0.1 μg/ml;定量限为0.3 μg/ml;114份样品中,共检出阳性样品29份,检出率为25.4%,含量为每贴1~47 mg,且阳性样品多集中在医用冷敷贴、远红外镇痛贴样品中.结论 该方法准确度高、快捷灵敏,适用于贴敷类医疗器械产品非法添加的水杨酸甲酯进行定性与定量分析.

Abstract

Objective To establish a rapid and novel analytical method using ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)for the qualitative and quantitative determination of illegally added methyl salicylate in topical medical devices.The samples were extracted with methanol,filtered,and then analyzed using UPLC-MS/MS.Methods The separation was performed on a WATERS ACQUITY UPLC BEH C18 column(2.1×100 mm,1.7 μm)with a gradient elution of 0.05%ammonia solution-methanol as the mobile phase.Electrospray ionization(ESI)in negative ion mode and multiple reaction monitoring(MRM)were used for data acquisition.Results The linear relationship of methyl salicylate was good within the range of 1~100 μg/ml,with a correlation coefficient of 0.9997.The average recovery rate of three spiked levels was 90.3%~100.7%,with a relative standard deviation(RSD)of 0.5%~0.9%.The limit of detection(LOD)of the method was 0.1 μg/ml,and the limit of quantitation(LOQ)was 0.3 μg/ml.Methyl salicylate was detected in 29 out of 114 samples,with a content ranging from 1 to 47 mg per patch.Conclusion This method is characterized by its high specificity,accuracy,speed,and sensitivity,and is suitable for the qualitative and quantitative determination of illegally added methyl salicylate in medical dressings.

关键词

贴敷类医疗器械/水杨酸甲酯/超高效液相色谱-串联质谱法

Key words

Medical dressings/Methyl salicylate/UPLC-MS/MS

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基金项目

江西省药品监督管理局科技项目(2022JS09)

出版年

2024
医疗装备
国家食品药品监督管理局北京医疗器械质量监督检验中心 北京市医疗器械检验所

医疗装备

影响因子:0.339
ISSN:1002-2376
参考文献量18
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