摘要
目的建立生脉饮中4种植物生长延缓剂残留量的检验检测方法。方法应用QuEChERS-超高效液相色谱-串联质谱(UPLC-MS/MS)技术,采用Welch ultimate LP-C18色谱柱(2.1 mm×100 mm,1.8μm),以乙腈-0.1%甲酸的5 mmol/L乙酸铵溶液(55∶45)为流动相,流速0.2 mL/min,柱温30℃,进样量为3μL,采用电喷雾正离子源(ESI+),多反应监测(MRM)模式。结果136批次样品中14批次检出多效唑,检出率为10.3%,含量范围为10.2~121.9 ng/mL,未检出丁酰肼、矮壮素、缩节胺。多效唑在5.39~431.2 ng/mL范围内与峰面积积分值线性关系良好(r=0.9975),平均加样回收率为93.3%,RSD为3.0%。结论该方法准确、简便、快速,可作为生脉饮中多效唑残留量的检验检测方法。
Objective To establish a method for the determination of four plant growth retardants residues in shengmaiyin.Methods Application of QuEChERS-UPLC-MS/MS technology,Welch ultimate LP-C18 column(2.1 mm×100 mm,1.8μm)was adopted,acetonitrile-0.1%formic acid 5 mmol/L ammonium acetate solution(55∶45)was used as mobile phase,the flow rate was 0.2 mL/min,the column temperature was 30℃,injection volume was 3μL,adopt electric spray ion source(ESI+)and multiple reaction monitoring(MRM)mode.Results Among 136 batches of samples,14 batches of paclobutrazol were detected,the detection rate was 10.3%,and the content range was 10.2-121.9 ng/mL,daminozide,chlormequat chloride and mepiquat chloride were not detected.The sample injection of paclobutrazol have a good linear relationship in 5.39-431.2 ng/mL(r=0.9975),the recovery rate was 93.3%,RSD was 3.0%.Conclusion This method is accurate,simple and fast,and can be used as the detection method for paclobutrazol residues in shengmaiyin.
作者
胡亮
周明
文庆
孙辉
丁野
罗疆南
HU Liang;ZHOU Ming;WEN Qing;SUN Hui;DING Ye;LUO Jiangnan(Hunan Institute of Drug Inspection and Testing,Hunan Engineering and Technology Research Center for Pharmaceutical Quality Evaluation,Changsha Hunan 410001,China;Hunan Drug Inspection Center,Changsha Hunan 410013,China;Hunan Drug Evaluation and Adverse Reaction Monitoring Center,Changsha Hunan 410013,China)
出处
《药品评价》
CAS
2023年第3期290-293,共4页
Drug Evaluation
关键词
农药残留量
生脉饮
QUECHERS
植物生长延缓剂
超高效液相色谱-串联质谱
安全监管
Pesticide residues
Shengmaiyin
QuEChERS
Plant growth retardant
Ultra high performance liquid chromatographytandem mass spectrometry(UPLC-MS/MS)
Safety supervision