摘要
建立妇科用医疗器械中甲硝唑识别及含量测定的高效液相色谱检测方法,并用高效液相色谱-四极杆飞行时间质谱对测定结果验证。选择Thermo Acclaim120 C18色谱柱(250 mm×4.6 mm,5μm)为分离柱,以甲醇-水为流动相进行梯度洗脱,检测波长为320 nm,柱温为30℃,进样体积为10μL,流量为1.0 mL/min。甲硝唑的质量浓度在2.6~257.2μg/mL范围内与色谱峰面积线性关系良好,相关系数0.999 9,方法检出限为0.05μg/mL,定量限为0.3μg/mL。卡波姆妇科洗液、医用妇科敷料凝胶样品的加标平均回收率分别为98.1%、98.8%,测定结果的相对标准偏差分别为0.19%、0.17%(n=6)。液相色谱-质谱验证结果表明,样品中相关分子离子峰及特征碎片离子峰与甲硝唑对照品一致。该方法可用于妇科用医疗器械中非法添加甲硝唑的质量控制。
A method of high-performance liquid chromatography was established for identifying and determining the content of metronidazole in gynecological medical devices,and validated the determination results by high performance liquid chromatography-quadrupole time-of-flight mass spectrometry.Thermo Acclaim120 C18 chromatographic column(250 mm×4.6 mm,5μm)was used as the separation column,performed gradient elution with methanol-water as the mobile phase.The detection wavelength was 320 nm,the column temperature was 30℃,and the injection volume was 10μL at the flow rate of 1.0 mL/min.The mass concentration of metronidazole had good linear relationship with the chromatographic peak area in the range of 2.6-257.2μg/mL,with the correlation coefficient of 0.9999.The detection limit of the method was 0.05μg/mL,and the quantification limit was 0.3μg/mL.The average recoveries of carbomer gynecological lotion and medical gynecological dressing gel were 98.1%and 98.8%,respectively.The relative standard deviations of the determination results for six parallel samples were 0.19%and 0.17%,respectively.The verification results of liquid chromatography-mass spectrometry showed that the relevant molecular ion peaks and characteristic fragment ion peaks in the sample were consistent with those of the metronidazole reference substance.This method can be used for quality control of illegally added metronidazole in gynecological medical devices.
作者
单如梦
王婷婷
陈乃江
李玲
王秋实
SHAN Rumeng;WANG Tingting;CHEN Naijiang;LI Ling;WANG Qiushi(Lianyungang Institute for Food and Drug Control,Lianyungang 222000,China)
出处
《化学分析计量》
2026年第1期68-74,共7页
Chemical Analysis And Meterage
基金
江苏省药品监督管理局药品监管科学科研计划项目(202369)
国家药品监督管理局药品补充检验方法项目(2023002)。
关键词
妇科用医疗器械
甲硝唑
高效液相色谱-四极杆飞行时间质谱法
高效液相色谱法
gynecological medical devices
metronidazole
high performance liquid chromatography-quadrupole time-of-flight mass spectrometry
high performance liquid chromatography
