高效液相色谱-串联质谱法测定凉茶中8种非法添加药物  

Determination of 8 adulterated drugs in herbal tea by high performance liquid chromatography-tandem mass spectrometry

作　　者：温家欣[1] 曹雅静 何嘉雯 钟常风 赖宇红[1] WEN Jiaxin;CAO Yajing;HE Jiawen;ZHONG Changfeng;LAI Yuhong(Guangdong Institute for Drug Control,Guangzhou 510663,China;Guangzhou Xinhua College,Guangzhou 510520,China)

机构地区：[1]广东省药品检验所,广东广州510663 [2]广州新华学院,广东广州510520

出　　处：《中国测试》2023年第6期62-67,共6页China Measurement & Test

基　　金：广东省医学科学技术研究基金(B2021300);广东省药品监督管理局科技创新项目(2022TDZ02,SN2022024)。

摘　　要：文章以临床常用、与感冒咳嗽适应症高度吻合的8种化学药物为研究对象,建立高效液相色谱-串联质谱同时测定多种非法添加化学药物的分析方法。样品经甲醇超声提取,以5 mmol/L甲酸铵溶液(含0.1%甲酸)–0.1%甲酸乙腈为流动相体系进行梯度洗脱,采用Agilent Poreshell EC-C18(100 mm×2.1 mm,2.7μm)色谱柱分离,外标法定量。8种目标化合物在线性范围内线性关系良好,相关系数均大于0.9993,方法检出限为0.01~0.3 mg/kg,方法定量限为0.025~1 mg/kg,基质效应系数的绝对值均小于18%。各目标化合物的平均回收率为65.0%~105.7%,重复性相对标准偏差(n=6)范围为1.6%~10.6%,24 h内进样精密度相对标准偏差均小于6%。该方法简单快速,灵敏度高,准确性、重复性和稳定性良好,填补现行标准的技术空白,可满足实际检验工作的需要。An analytical method for the simultaneous determination of adulterants by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)was established for 8 kinds of chemical drugs,which were commonly used in clinic and highly consistent with the indications of cold and cough.The samples were extracted by ultrasonic extraction with methanol and eluted by gradient elution using 5 mmol/L ammonium formate solution(containing 0.1%formic acid)–0.1%formic acid acetonitrile as mobile phase system.The separation was performed on an Agilent Poreshell EC-C18 column(100 mm×2.1 mm,2.7μm),and quantified by external standard method.The 8 target compounds showed good linear relationships within their respective linear ranges,with correlation coefficients(R)great than 0.9993.The limits of detection(LODs)ranged from 0.01 mg/kg to 0.3 mg/kg,the limits of quantification(LOQs)ranged from 0.025 mg/kg to 1 mg/kg,and the absolute values of matrix effect coefficients(MEs)were all less than 18%.The average recoveries of the target compounds ranged from 65.0%to 105.7%,and the relative standard deviations(RSDs,n=6)of repeatability ranged from 1.6%to 10.6%,and the relative standard deviations of injection precision within 24 h were all less than 6%.The method is simple,rapid,sensitive,accurate,repeatable and stable,which meets the requirements of quantitative analysis and can meet the needs of practical inspection.

关 键 词：凉茶 非法添加 抗病毒类药物 镇咳祛痰类药物 抗组胺类药物 

分 类 号：TB9[一般工业技术—计量学]