测定人参花中多种有机氯农药残留量的方法研究

Determination of organochlorine pesticide residues in ginseng flower by gas chromatography

建立一种测定人参花中16种有机氯类农药残留量的方法,并对其进行方法学考察。方法样品经乙腈提取后,加入无水硫酸镁和氯化钠除水、分层,再通过N-丙基乙二胺(PSA)、十八烷基硅烷键合硅胶(C18)和无水硫酸镁净化,浓硫酸除水、脱色,采用气相色谱法测定,外标法定量。16种有机氯农药在质量浓度0.001~0.100μg·mL^(-1)范围内均呈现良好的线性关系,相关系数r≥0.99914,且分离度良好;检出限(LOD)为0.00026~0.00073μg·mL^(-1),定量限(LOQ)为0.00080~0.0022μg·mL^(-1);人参花样品在0.0050、0.010、0.050、0.100 mg·kg^(-1)添加水平下的回收率为77.20%~116.87%;相对标准偏差(RSD)在1.31%~11.88%,符合农药残留相关分析标准<15%的要求。本实验所建立的方法简便快速、灵敏度高,适用于人参花中16种有机氯农药残留量的同时测定。

To establish a method for the determination of 16 organochlorine pesticides residues in ginseng flower and its methodology was investigated.Method After the sample is extracted by acetonitrile,anhydrous magnesium sulfate and sodium chloride are added to remove water and layer,and then purified by N-propylethylenediamine(PSA),octadecylsilane bonded silica gel(C18)and anhy-drous magnesium sulfate.The concentrated sulfuric acid is removed from water and decolored,determined by gas chromatography,and quantified by external standard method.All the 16 organochlorine pesticides showed good linear relationship in the concentra-tion range of 0.001~0.100μg mL^(-1),the correlation coefficient r≥0.99914,and the separation degree was good;The limits of de-tection(LOD)were 0.00026~0.00073μg·mL^(-1),and the limits of quantitation(LOQ)were 0.00080~0.0022μg·mL^(-1).The re-coveries of ginseng flower samples at 0.0050,0.010,0.050 and 0.100 mg·kg^(-1)l were 77.20%~116.87%.The relative standard deviation(RSDS)was between 1.31%and 11.88%,which met the requirement of pesticide residue correlation analysis standard<15%.The method is simple,rapid,sensitive and suitable for the simultaneous determination of 16 organochlorine pesticides residues in panax ginseng flowers.