QuEChERS-高效液相色谱法测定铁皮石斛中多菌灵和甲基硫菌灵的残留量  

Determination of Carbendazim and Thiophanate-methyl in Dendrobium officinale by QuEChERS-HPLC

作　　者：陈思颖[1,2,3] 吴耽[1,4] 巩仔鹏 谭丹 孙佳[1,2] 杨畅 CHEN Siying;WU Dan;GONG Zipeng;TAN Dan;SUN Jia;YANG Chang(Guizhou Provineial Key Laboratory of Pharmaceutics,Guizhou Medical University,Guiyang 550004,Guizhou,China;Engineering Research Center for the Development and Application of Ethnic Medicine and TCM,Ministry of Education,Guiyang 550004,Guizhou,China;National Engineering Researeh Center of Miao ＇ s Medicines,Guiyang 550004,Guizhou,China;School of Pharmacy,Guizhou Medical University,Guiyang 550004,Guizhou,China)

机构地区：[1]贵州医科大学贵州省药物制剂重点实验室,贵州贵阳550004 [2]民族药与中药开发应用教育部工程研究中心,贵州贵阳550004 [3]国家苗药工程技术研究中心,贵州贵阳550004 [4]贵州医科大学药学院,贵州贵阳550004

出　　处：《贵州医科大学学报》2018年第8期913-917,共5页Journal of Guizhou Medical University

基　　金：贵州省中药现代化科技产业研究开发项目[黔科合SY字(2014)3032-2号];民族药与中药开发应用产学研基地建设项目[黔科合KY字(2013)122];民族药化学成分及活性研究[黔科合人字(2015)11号]

摘　　要：目的:建立QuEChERS-高效液相色谱法测定不同产地铁皮石斛中多菌灵与甲基硫菌灵农药残留量的方法。方法:铁皮石斛样品用乙腈溶液提取,经QuEChERS方法净化,采用Waters C_(18)色谱柱(150 mm×4.6mm,5μm)、乙腈-0.02 mol/L乙酸铵缓冲溶液(20∶80)为流动相,流速1 mL/min、柱温35℃、检测波长280 nm,对不同产地铁皮石斛中多菌灵与甲基硫菌灵残留量进行检测。结果:多菌灵在0.05~25 mg/L范围内呈良好的线性关系,相关系数等于0.999 4,检测限为0.01 mg/kg,定量限为0.04 mg/kg,3个添加水平下的平均回收率是98.28%,RSD是2.68%;甲基硫菌灵在0.025~12.5 mg/L范围内呈良好的线性关系,相关系数等于0.999 5,检测限为0.02 mg/kg,定量限为0.06 mg/kg,3个添加水平下的平均回收率是101.03%,RSD是3.64%;50批铁皮石斛中有4批分别检出多菌灵与甲基硫菌灵农药残留,均低于《中国药典》2015年版中药有害残留物限量制定指导原则农药残留量最大限量理论值。结论:建立的QuEChERS-高效液相色谱法检测多菌灵和甲基硫菌灵,具有操作简单,高效、专属性好、重复性强、结果准确可靠等优点。Objective： To establish a method for simultaneous determination of residual carbendazim and thiophanate-methyl in Dendrobium officinale from different regions by QuEChERS-HPLC. Methods： The samples were extracted by acetonitrile and purified by the optimized QuEChERS method.Then the carbendazim and thiophanate-methyl residues in Dendrobium officinale from different regions were determined by HPLC method with Waters C18 column（ 150 mm × 4. 6 mm,5 μm）. The mobile phase was acetonitrile-0. 02 mol/L ammonium acetate buffer for isogradient elution（ 20∶ 80）. The flow rate was 1 m L·min-1. The column temperature was 35 ℃ and the detection wavelength was 280 nm.Results： When the concentrations ranged from 0. 05 to 25 mg/L,the linear relationship was good（ r =0. 999 4） in the case of with carbendazim. The detection limit was 0. 01 mg/kg,the quantitative limit was 0. 04 mg/kg,and the average recovery and RSD under three different levels of addition were98. 28% and 2. 68%; When the concentrations ranged from 0. 025 to 12. 5 mg/L,the linear relationship was also good（ r = 0. 999 5） in the case with thiophanate-methyl. The detection limit was 0. 02 mg/kg,the quantitative limits was 0. 06 mg/kg,and the average recovery and RSD under three different levels of addition were 101. 03% and 3. 64%. The residue of carbendazim and thiophanate-methyl were detected in 4 batches among 50 batches of Dendrobium officinale,but lower than the theoretical value of maximum limit of pesticide residue in the guideline for the limitation of harmful residues of traditional Chinese medicine from China Pharmacopeia（ 2015 edition）. Conclusion： The Qu ECh ERHPLC method was established for the determination of carbendazim and thiophanate-methyl in the Dendrobium officinale. This method is simple and efficient with good specificity and strong repeatability.The results are accurate and reliable,providing real and effective basis for the quality control of Dendrobium candidum.

关 键 词：植物 药用 铁皮石斛 色谱法 高效液相 多菌灵 甲基硫菌灵 

分 类 号：R932[医药卫生—生药学]