气相色谱-串联质谱测定川芎中65种农药残留

Determination of 65 pesticide residues in Chuanxiong Rhizoma by GC-MS/MS

目的:建立了QuEChERS技术结合气相色谱-串联质谱(GC-MS/MS)同时检测川芎中65种农药残留的快速分析方法,并对38批来自市场和不同产地的川芎进行初步筛查。方法:川芎样品加水经乙腈提取,以QuEChERS提取包(含无水硫酸镁与无水乙酸钠等)进行盐析,提取液经浓缩后,加入内标磷酸三苯酯,采用GC-MS/MS进行检测分析。色谱-质谱条件:采用Agilent DB17-MS色谱柱(30.0 m×0.25mm×0.25μm),载气为高纯氦气,进样量1μL,高压不分流进样,柱流速为线速度控制模式,初始流速为1.3mL·min-1,进样口温度为240℃,动态多反应监测模式(MRM),离子源温度200℃,接口温度280℃。结果:65种农药在一定含量范围内线性关系良好,相关系数(r)均大于0.9987,在3个添加水平下,回收率在60%~140%范围内的农药数占总数的93.85%,92.31%的农药RSD小于15%。对收集到的38批川芎样品进行检测,共检出6种农药,其中毒死蜱检出率高达81.58%。结论:该方法简便、灵敏、准确,可用于川芎中多种农药残留的快速筛查与检测,可为川芎的种植生产和质量管控提供技术支撑。

Objective:To establish a rapid analysis method of QuEChERS technology combined with gas chromatography-tandem mass spectrometry(GC-MS/MS)to detect 65 pesticide residues in Chuanxiong Rhizoma,and to screen 38 batches of ligusticum chuanxiong samples from different markets and different origins.Methods:Chuanxiong Rhizoma was treated with water and extracted with acetonitrile,and the QuEChERS package(containing anhydrous magnesium sulfate and anhydrous sodium acetate,etc.)was used for salting out.After the extraction solution was concentrated,internal standard triphenyl phosphate was added,and GC-MS/MS was used for detection and analysis.Chromatography-mass spectrometry conditions are as to Uows:Elastic quartz capillary column(30.0 m×0.25 mm×0.25μm)DB17-MS was used,high purity helium was sued as carrier gas,injection volume was 1μL,linear velocity control mode was used to control column velocity,the initial velocity of 1.3 mL·min-1.The inlet temperature was 240℃.Dynamic multi-reaction monitoring mode(MRM)was used.Ion source temperature was 200℃and the interface temperature was 280℃.Results:All there a good linear relationship within certain content ranges for 65 pesticides,with the correlation coefficients(r)greater than 0.9987.Under the three addition levels,the recovery range were within 60%-140%for 93.85%of 65 pesticides,and for 92.31%of the pesticides the relative standard deviation was less than 15%.Thirty-eight batches of chuanxiong samples were tested and six pesticides were detected.The detection rate of chlorpyrifos was 81.58%.Conclusion:This method is simple,sensitive and accurate,which can be used for rapid screening and detection of various pesticide residues in Chuanxiong Rhizoma,and can provide technical support for the cultivation,production and quality control of Chuanxiong Rhizoma.