混合型固相萃取-亲水作用色谱串联质谱法测定熊胆粉中7种氨基糖苷类抗生素残留量  

Determination of 7 aminoglycoside antibiotics residues in bear bile powder by mix-mode SPE-hydrophilic interaction liquid chromatography tandem mass spectrometry

作　　者：胡青 孙健 于泓 张静娴 毛秀红 季申 HU Qing;SUN Jian;YU Hong;ZHANG Jing-xian;MAO Xiu-hong;JI Shen(China State Institute of Pharmaceutical Industry,Shanghai 201203,China;NMPA Key Laboratory for Quality Control of Traditional Chinese Medicine,Shanghai Institute for Food and Drug Control,Shanghai 201203,China)

机构地区：[1]中国医药工业研究总院,上海201203 [2]上海市食品药品检验研究院,国家药品监督管理局中药质量控制重点实验室,上海201203

出　　处：《药学学报》2022年第12期3621-3625,共5页Acta Pharmaceutica Sinica

基　　金：国家中药标准化项目(ZYBZH-C-SH-48);上海市自然科学基金资助项目(19ZR1448300)。

摘　　要：建立了亲水作用色谱串联三重四极杆质谱测定熊胆粉中7种氨基糖苷类抗生素的方法。采用混合型弱阳离子交换反相吸附固相萃取净化样品,Waters ACQUITY UPLC BEH Amide色谱柱(100 mm×3.0 mm,1.7μm),以0.2%甲酸水溶液-0.2%甲酸乙腈溶液为流动相,梯度洗脱,在电喷雾离子化正离子模式下,以多反应监测方式(MRM)检测。大观霉素、链霉素、丁胺卡那霉素、卡那霉素、妥布霉素、安普霉素、新霉素在各自浓度范围内均呈良好线性关系,相关系数均在0.99以上;三水平平均加样回收率为61.3%~127.3%,相对标准偏差(RSD)为0.1%~1.9%;定量限为0.2~1.0 mg·kg^(-1)。本方法已应用于实际样品的测定。An analytical method was developed for determination of 7 aminoglycosides antibiotics in bear bile powder by hydrophilic interaction liquid chromatography tandem mass spectrometry.The samples were purified by mix-mode weak cation exchange and reversed-phase SPE.Waters ACQUITY UPLC BEH Amide column(100 mm×3.0 mm,1.7μm)was used with 0.2%formic acid aqueous solution-0.2%formic acid acetonitrile solution as mobile phases by gradient elution.The aminoglycosides were detected by electrospray ionization mass spectrometry in positive mode with multiple reaction monitoring(MRM)mode.Spectinomycin,streptomycin,amikacin,kanamycin,tobramycin,apramycin and neomycin possessed good linear correlation in the respective concentration ranges,with the correlation coefficients more than 0.99.The mean recoveries at 3 spiked levels were in the range of 61.3%~127.3%,and the RSDs were 0.1%~1.9%.The limits of quantification were 0.2~1.0 mg·kg^(-1).The method had been applied to the analysis of actual samples.

关 键 词：亲水作用色谱串联质谱 混合型固相萃取 熊胆粉 氨基糖苷 

分 类 号：R917[医药卫生—药物分析学]