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建立了中药材三七中农药残留分析的两种样品前处理方法,在样品前处理方法 I中,样品经正己烷与二氯甲烷(体积比为6∶4)混合溶剂超声提取,提取液经Envi-carb/NH2SPE小柱净化;在样品前处理方法Ⅱ中,采用基质固相分散萃取净化法对样品进行提取净化。两种方法所得到的洗脱液,于旋转蒸发仪上浓缩近干,二氯甲烷定容后于气相色谱质谱(GC-MS)检测。采用GC-MS的选择离子监测(SIM)方式和外标法定量。在优化的样品前处理条件和GC-MS分析条件下,方法简便、快速,添加水平为0.01、0.5和2.0 mg·kg-1进行加标回收率实验时,采用方法Ⅰ时的回收率为81.90%~102.10%,相对标准偏差(RSD)为3.60%~7.10%;采用方法Ⅱ时的回收率为96.26%~104.20%,RSD为3.52%~7.94%;检出限在0.48~1.34 ng·g-1之间。两种前处理方法的各项技术指标满足农药残留检测要求,适合三七样品中痕量农药残留的分析。
Two sample pretreatment methods were established for the analysis of pesticide residues in Panax notoginseng. In sample preparation method I, the sample was extracted with a mixed solvent of n-hexane and dichloromethane (volume ratio of 6: 4) Envi-carb / NH2SPE cartridge purification; Sample Pretreatment Ⅱ, the use of matrix solid phase dispersion extraction and purification of the sample extraction and purification. The eluent obtained by the two methods was concentrated to near dryness on a rotary evaporator, and the volume of methylene chloride was determined by gas chromatography-mass spectrometry (GC-MS). Selected by GC-MS ion monitoring (SIM) method and external standard method. Under the optimal conditions of sample preparation and GC-MS analysis, the method was simple and rapid, and the recoveries of spiked samples at 0.01, 0.5 and 2.0 mg · kg-1 were 81.90 The relative standard deviations (RSDs) ranged from 3.60% to 7.10%. The recoveries were 96.26% -104.20% with RSD 3.52% -7.94% when the method Ⅱ was used. The detection limits were between 0.48 and 1.34 ng · g -1 between. The two pretreatment methods of the technical indicators to meet the requirements of pesticide residue detection, suitable for analysis of trace pesticide residues in the sample.