摘要
目的建立麦冬中金属及有害元素与农药残留的测定方法。方法采用电感耦合等离子体-质谱法测定麦冬药材中16种金属及有害元素的含量,射频功率为1300 W,氩气流速为15.0 L/min,辅助气流速为0.10 L/min,雾化气流速为0.9 L/min,采样深度为7.0 mm,采样锥孔径为1.0 mm,雾室温度为2℃。采用气相色谱串联质谱法测定麦冬药材中30种农药残留量,色谱柱为HP-5MS毛细管柱(30 m×0.25 mm,0.25μm),进样口温度为240℃,进样方式为不分流,载气为高纯度氦气,恒压模式,流速为1.3 m L/min,进样量为1μL,程序升温;离子源为电子轰击源;监测模式为多反应监测模式,离子源温度为230℃,质谱传输接口温度为280℃,碰撞气体为氩气;溶剂延迟时间为1.5 min。结果硼(B)、铝(Al)、铁(Fe)、铜(Cu)质量浓度均在0~200μg/L,钪(Sc)、镍(Ni)、锌(Zn)、砷(As)、硒(Se)、锶(Sr)、镉(Cd)、锡(Sn)、碲(Te)、钡(Ba)、铅(Pb)质量浓度均在0~40μg/L,汞(Hg)质量浓度在0~8μg/L范围内与仪器信号强度线性关系良好(r>0.995);重复性试验的RSD均小于4.10%(n=9);平均加样回收率均为87.01%~102.41%,RSD均为1.21%~4.41%(n=9)。α-六六六、β-六六六、γ-六六六、特丁硫磷、δ-六六六、三氯杀螨醇、p,p'-DDE、p,p'-DDD、o,p'-DDT、内吸磷、灭线磷、氟甲腈、甲基异柳磷、氟虫腈亚砜、氟虫腈砜质量浓度均在5~200 ng/m L,甲基对硫磷、艾氏剂、对硫磷、氟虫腈、除草醚、甲拌磷、水胺硫磷、特丁硫磷亚砜、特丁硫磷砜质量浓度均在10~200 ng/m L,杀虫脒质量浓度在15~200 ng/m L,α-硫丹、β-硫丹、久效磷质量浓度均在20~200 ng/m L,蝇毒磷质量浓度在30~200 ng/m L,狄氏剂质量浓度在35~200 ng/m L范围内与峰面积线性关系良好(r>0.994);检测限均为0.005~0.025 mg/kg;精密度试验结果的RSD均小于6.22%(n=9);平均回收率均为70.50%~89.33%,RSD均为1.41%~9.45%(n=9)。12批药材样品中铝含量为41.98~423.74 mg/kg,铁含量为67.76~321.7
Objective To establish a method for the determination of metal elements,harmful elements and pesticide residues in Ophiopogon japonicus.Methods The contents of 16 metal elements and harmful elements in Ophiopogon japonicus were determined by inductively coupled plasma-mass spectrometry(ICP-MS),the radio frequency(RF)power was 1300 W,the flow rate of argon was 15.0 L/min,the flow rate of auxiliary gas was 0.10 L/min,the flow rate of atomization gas was 0.9 L/min,and the sampling depth was 7.0 mm,the diameter of sampling cone was 1.0 mm,and the temperature of fog chamber was 2℃.A total of 30 pesticide residues in Ophiopogon japonicus were determined by the gas chromatography-tandem mass spectrometry(GC-MS/MS)method.The chromatographic column was HP-5 MS capillary column(30 m×0.25 mm,0.25μm),the temperature of the injection port was 240℃,the splitless injection mode was adopted,the carrier gas was high-purity helium,the constant pressure mode was adopted,the flow rate was 1.3 m L/min,the injection volume was 1μL,programmed-temperature was adopted,the ion source was electron bombardment source,the monitoring mode was multiple reaction monitoring mode,the temperature of ion source was 230℃,the temperature of mass spectrometry transmission interface was 280℃,the collision gas was argon,and the solvent delay time was 1.5 min.Results The mass concentration of boron(B),aluminum(Al),iron(Fe),copper(Cu)showed a good linear relationship with the signal intensity of the instrument in the range of 0-200μg/L,the mass concentration of scandium(Sc),nickel(Ni),zinc(Zn),arsenic(As),selenium(Se),strontium(Sr),cadmium(Cd),tin(Sn),tellurium(Te),barium(Ba)and lead(Pb)showed a good linear relationship with the signal intensity of the instrument in the range of 0-40μg/L,the mass concentration of mercury(Hg)showed a good linear relationship with the signal intensity of the instrument in the range of 0-8μg/L(r>0.995).The RSD of the repeatability test was less than 4.10%(n=9).The average recoveries of 16 metal elements and har
作者
苏建
刘永利
SU Jian;LIU Yongli(Laboratory for Inspection of Traditional Chinese Medicine,Hebei Institute for Drug and Medical Device Control·NMPA Key Laboratory for Quality Monitoring and Evaluation of Traditional Chinese Medicine<Chinese Materia Medica>,Shijiazhuang,Hebei,China 052000)
出处
《中国药业》
CAS
2021年第16期75-81,共7页
China Pharmaceuticals
基金
河北省中医药管理局科研计划项目[2014182]。
