固相萃取与高效液相色谱法联用检测人参中的8种杀菌剂

Determination of Eight Fungicides Residues in Ginseng by HPLC Coupled with Solid Phase Extraction

【目的】建立以固相萃取法（SPE）和高效液相色谱法（HPLC）联用技术检测人参中的8种杀菌剂（甲霜灵、烯酰吗啉、咯菌腈、嘧霉胺、氟硅唑、嘧菌环胺、醚菌酯、氟菌唑）的检测方法。[方法】人参样品用正己烷饱和的乙腈提取，在经过串联的GPR和LC—Florisil固相萃取柱净化，然后采用反相HPLC测定，外标法定量。对样品前处理和色谱分离条件进行了研究和优化。【结果】8种杀菌剂在0．2～5．0mg／L范围内线性关系良好，相关系数为0．9948~0．9999。在0．1、0．2、0．5mg／kg三个添加水平上，回收率范围为75．0％～106．0％，相对标准偏差为2．5％-9．7％。【结论】该方法简单、快速、灵敏、可靠，净化效果较好，可用于人参中多种杀菌剂残留量的同时测定。

[Aims] A testing method was developed using solid phase extraction （SPE） for cleaning-up and high performance liquid chromatography （HPLC） for simultaneous analysis of eight fungicides residues （metalaxyl, dimethomorph, fludioxonil, pyrimethanil, flusilazole, cyprodinil, kresoxim-methyl and triflumizole） in ginseng. [Methods] Homogenized ginseng samples were extracted with acetonitrile （saturated by n-hexane）, and purified by a GPR coupled with a LC-Florisil solid phase extraction cartridge, then analyzed by reversed-phase HPLC with external standard method. Sample preparation and chromatographic separation conditions were studied and optimized. [Results] The calibration curves of the eight fungicides were linear enough in the concentrations from 0.2- 5.0 mg/L with the correlation coefficients in the range of 0.994 8-0.999 9. The recoveries from spiked samples at the three levels of 0.1, 0.2, 0.5 mg/kg are between 75.0 and 106.0% with relative standard deviations ranged from 2.5 to 9.7%. [Conclusions] This method is simple, rapid, sensitive, reliable, and efficient with good cleaning-up effect, which can be used to simultaneously detect multi-fungicides residues in ginseng.