摘要
目的采用UPLC-MS/MS法同时测定四大怀药(怀山药、怀地黄、怀牛膝、怀菊花)中19种植物生长调剂的残留量。方法采用Capcell PAK强阳离子交换与C_(18)混合填料色谱柱(15 cm×2.0 mm,5μm),以0.1%甲酸溶液(5 mmol·L^(-1)甲酸铵)为流动相A,乙腈-0.1%甲酸溶液(5 mmol·L^(-1)甲酸铵)(95:5)为流动相B,梯度洗脱,流速为0.3 mL·min^(-1),柱温40℃。结果19种植物生长调节剂的线性均良好(r>0.9900),检出限为0.05~19.35 ng·mL^(-1);平均回收率为79%~105%,RSD为0.78%~13.40%(n=6)。结论所用方法准确、快速、灵敏,可用于怀山药、怀地黄、怀牛膝、怀菊花中19种植物生长调节剂的定性及定量残留检测。
OBJECTIVE To establish an UPLC-MS/MS method for the simultaneous determination of 19 plant growth regulator residues in Huai Dioscoreae Rhizoma,Huai Rehmanniae Radix,Huai Achyranthis bidentatae Radix and Huai Chrysanthemi Flos,known as four major Huaiqing Chinese medicines.METHODS A Capcell PAK cation exchange mixed C_(18)column(15 cm×2.0 mm,5μm)was used,with 0.1%formic acid solution(5 mmol·L^(-1)ammonium formate)as mobile phase A and acetonitrile-0.1%formic acid solution(5 mmol·L^(-1)ammonium formate)(95:5)as mobile phase B,and gradient elution was carried out at a flow rate of 0.3 mL·min^(-1),and column temperature of 40℃.RESULTS The 19 plant growth regulator residues showed good linearity,with determination limits of 0.05-19.35 ng·mL^(-1)and r>0.9900,respectively.At three different mass fraction levels,the average recovery rates were in the range of 79%-105%,with the RSDs of 0.78%-13.40%(n=6),respectively.CONCLUSION This method is accurate,rapid and sensitive,which can be used for the residue identification and content determination of 19 plant growth regulators in Huai Dioscoreae Rhizoma,Huai Rehmanniae Radix,Huai Achyranthis bidentatae Radix and Huai Chrysanthemi Flos.
作者
李逢春
杨元
李海燕
王海波
LI Fengchun;YANG Yuan;LI Haiyan;WANG Haibo(NMPA Key Laboratory for Quality Control of Traditional Chinese Materia Medica and Prepared Slices,Henan Institute for Drug and Medical Device Inspection,Zhengzhou,Henan,450018 P.R.China)
出处
《华西药学杂志》
CAS
CSCD
北大核心
2024年第5期575-580,共6页
West China Journal of Pharmaceutical Sciences
基金
河南省科技攻关项目(202102310516)。
关键词
四大怀药
怀山药
怀地黄
怀牛膝
怀菊花
植物生长调节剂
残留
超高效液相色谱-串联质谱法
Four major Huaiqing Chinese medicine
Huai Dioscoreae Rhizoma
Huai Rehmanniae Radix
Huai Achyranthis bidentatae Radix
Huai Chrysanthemi Flos
Plant growth regulator
Residue
UPLC-MS/MS