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

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(2.1mm×100mm,1.7μm)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1~100μg/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0.1μg/ml;定量限为0.3μg/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1~47mg,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。

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,1.7μm)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 1~100μg/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 0.1μg/ml,and the limit of quantitation(LOQ)was 0.3μg/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.