摘要
目的建立广藿香中6种成分的质量分数测定方法及46种农药残留的液质联用检测方法,增加广藿香的质量评价指标。方法质谱采用电喷雾(ESI)离子源,正离子和负离子扫描模式,多反应监测模式(multiple reaction monitoring mode,MRM);液相采用Waters Acquity UPLC HSS T3柱(2.1 mm×100 mm,1.8μm);6种成分质量分数测定以甲醇(A)-0.1%(φ)甲酸(B)为流动相进行梯度洗脱,进样量为1μL,柱温为40℃,流速为0.2 mL/min;农药残留量检测的流动相为[甲醇-0.1%甲酸(含5 mmol/L甲酸铵)(体积比95∶5),A]-[0.1%甲酸(含5 mmol/L甲酸铵),B]梯度洗脱,柱温为40℃,流速为0.3 mL/min,。结果广藿香中6种成分呈良好的线性关系(r≥0.9977),平均回收率为98.6%~103.4%,RSD值为1.1%~1.8%;46种农药的线性关系良好(r≥0.9950);平均回收率为79.0%~106.2%,RSD为2.4%~9.9%。结论建立的方法灵敏度和准确度高、分析时间短,可用于检测广藿香中6种成分的质量分数和46种农药的残留量。建议将新西兰牡荆苷-2、毛蕊花糖苷、异毛蕊花糖苷、藿香黄酮醇、雷杜辛黄酮醇的质量分数和农药残留量作为指标纳入广藿香质量控制和质量评价体系。
Objective To establish mass fraction determination methods for 6 components in Patchouli and liquid chromatography-mass spectrometry detection methods for 46 pesticide residues,and add quality evaluation indicators for Patchouli.Methods The mass spectrometry conditions were electrospray ion source,positive and negative ion scanning mode,and multiple reaction monitoring mode(MRM).Waters Acquity UPLC HSS T3 column(2.1 mm×100 mm,1.8μm)was used.The mass fractions of six components were determined using a mobile phase of methanol-0.1%formic acid solution.The injection volume was 1μL,the column temperature was 40℃,and the flow rate was 0.2 mL/min.The mobile phase for pesticide residue detection was[(methanol-0.1%formic acid solution(containing 5 mmol/L ammonium formate)(95∶5),A]-[0.1%formic acid(containing 5 mmol/L ammonium formate),B]at gradient elution,with a column temperature of 40℃and a flow rate of 0.3 mL/min.Results The six components in patchouli showed a good linear relationship(r≥0.9977),with an average recovery rate of 98.6%to 103.4%and RSD values of 1.1%to 1.8%.The linear relationship of 46 pesticides was good(r≥0.9950),with an average recovery rate of 79.0%to 106.2%,and the RSD of 2.4%to 9.9%.Conclusion The established method has high sensitivity and accuracy,short analysis time,which can be used to simultaneously detect the content of 6 components and 46 pesticide residues in patchouli.It is recommended to bring the content of vicenin-2,verbascoside,isoverbascoside,pachypodol and retusin into the quality control and evaluation system of patchouli as indicators.
作者
朱小凤
黄少宏
黄婉锋
关倩怡
江珊
张艳萍
罗干明
ZHU Xiaofeng;HUANG Shaohong;HUANG Wanfeng;GUAN Qianyi;JIANG Shan;ZHANG Yanping;LUO Ganming(Foshan Center for Food and Drug Control,Foshan 528000,China;Jiangmen Institute for Drug Control,Jiangmen 529000,China)
出处
《广东药科大学学报》
2025年第6期73-83,共11页
Journal of Guangdong Pharmaceutical University
基金
佛山市科学技术局自筹经费类科技创新项目(2220001005638)。
