摘要
目的建立同时测定知母药材中8种植物生长调节剂残留量的超高效液相色谱-串联质谱法。方法色谱柱为Waters ACQUITY UPLC HSS T_(3)(2.1 mm×100 mm,1.8μm),柱温为30℃;流动相为5 mmol·L^(-1)甲酸铵溶液-乙腈(梯度洗脱),流速为0.3 mL·min^(-1),采用电喷雾离子源、多反应监测及正负离子模式采集数据。结果丁酰肼、矮壮素、助壮素、赤霉素、4-硝基苯酚钠、氯吡脲、多效唑、烯效唑在各自范围内呈良好的线性关系,r均>0.9991,检出限为0.001~0.03 ng·mL^(-1),平均加样回收率74.4%~113.8%,RSD<3%。30批次知母样品中有2批次检出矮壮素,含量分别为6.3和3.8μg·kg^(-1)。结论该方法操作简单、灵敏度高,可用于检测知母药材中植物生长调节剂残留量。
Objective To establish a simultaneous determination method for 8 plant growth regulator residues in Rhizoma Anemarrhenae by ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS-MS).Methods The separation was achieved on a Waters ACQUITY UPLC HSS T_(3) column(2.1 mm×100 mm,1.8μm)with a gradient elution of 5 mmol·L^(-1)ammonium formate solution(A)-acetonitrile(B)at a flow rate of 0.3 mL·min^(-1),and the column temperature was 30℃.The samples were detected by electrospray ionization(ESI)in positive/negative modes and multiple reaction monitoring mode.Results The linear relationships of daminozide,chlormequat,mepiquat,gibberellic acid,4-nitrophenol sodium salt dehydrate,forchlorfenuron,paclobutr azol,uniconazole were good in the selected concentration range,and the correlation coefficients were all greater than 0.9991.The detection limit were from 0.001 to 0.03 ng·mL^(-1).The average recoveries were from 74.4%to 113.8%,and the RSDs were less than 3%.Among the 30 batches of sibling samples,chlormequat chloride was detected in 2 batches,and their contents were 6.3 and 3.8μg·kg^(-1),respectively.Conclusion The method is simple e and high sensitive which can be used to detect the plant growth regulators residues in Rhizoma Anemarrhenae.
作者
黄晓婧
曾桢
肖春霞
许莉
李庆
赵小勤
HUANG Xiaojing;ZENG Zhen;XIAO Chunxia;XU Li;LI Qing;ZHAO Xiaoqin(Chengdu Institute for Drug Control/NMPA Key Laboratory for Quality Monitoring and Evaluation of Traditional Chinese Medicine(Chinese Materia Medica),Chengdu 610045,China)
出处
《医药导报》
CAS
北大核心
2022年第3期383-388,共6页
Herald of Medicine
基金
2017年国家药品计划抽验项目(食药监办药化监<2017>15号,中央补助地方经费项目)
四川省重大课题专项(2018TZDZX0007)。
