摘要
提出了高效液相色谱-串联质谱法同时测定中药材专用膨大剂类农肥中21种植物生长调节剂含量的方法。取农肥样品0.1 mL,经10 mL 50%(体积分数)乙腈溶液提取,150 mg MgSO_(4)和50 mg C_(18)吸附剂净化;在上清液中加入内标,涡旋、过滤后,取续滤液注入高效液相色谱-串联质谱仪。采用Agilent Poroshell 120 EC C_(18)色谱柱,以0.1%(体积分数)甲酸溶液-乙腈为流动相体系进行梯度洗脱;在电喷雾离子源正、负离子模式下,采用多反应监测模式检测,内标法定量。结果表明:21种植物生长调节剂的质量浓度在一定范围内与峰面积比值呈线性关系,检出限为0.01~4.00μg·kg^(-1),日内、日间测定值的相对标准偏差均小于5.0%;按照标准加入法进行回收试验,回收率为71.6%~105%。
A method for the simultaneous determination of 21 plant growth regulators in swelling agent type agricultural fertilizer used for traditional Chinese medicine by high performance liquid chromatography-tandem mass spectrometry was proposed.The agricultural fertilizer sample(0.1 mL)was taken,and 10 mL of 50%(volume fraction)acetonitrile solution was added for extraction.Then 150 mg of MgSO_(4)and 50 mg of C_(18)adsorbents were used for purification,and the internal standard was added into the supernatant.After vortex and filtration,the subsequent filtrate was injected into the high performance liquid chromatograph-tandem mass spectrometer.Gradient elution was performed on Agilent Poroshell 120 EC C_(18)column with 0.1%(volume fraction)formic acid solution-acetonitrile as mobile phase system.The multiple reaction monitoring mode was used for detection on the positive and negative mode of electrospray ionization source,with internal standard method for quantification.As shown by the results,linear relationships between the mass concentrations of 21 plant growth regulators and the peak area ratios were kept in definite ranges,with detection limits in the range of 0.01-4.00μg·kg^(-1),and RSDs of the determined values less than 5.0%.Test for recovery was made according to the standard addition method,giving results in the range of 71.6%-105%.
作者
韩佳
罗祖良
马小军
臧艺玫
谢林辰
厉妲
HAN Jia;LUO Zuliang;MA Xiaojun;ZANG Yimei;XIE Linchen;LI Da*(School of Biomedicine,Beijing City University,Beijing 100094,China;Institute of Medicinal Plant Development,Chinese Academy of Medical Sciences&Peking Union Medical College,Beijing 100193,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2024年第4期398-403,共6页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
中央高校基本科研业务费专项资金(3332020047)
研究生科研创新项目(Yjscx202139)
北京城市学院发展基金(KYFZ202101)。
关键词
高效液相色谱-串联质谱法
农肥
植物生长调节剂
中药材
high performance liquid chromatography-tandem mass spectrometry
agricultural fertilizer
plant growth regulator
traditional Chinese medicine
