SPE-HPLC紫外双波长测定水果中10种农药残留

Determination of 10 Pesticide residues in Fruits by HPLC with SPE and UV Double Wavelength

建立了固相萃取（SPE）-高效液相色谱（HPLC）紫外检测器双波长同时测定草莓、桃和苹果中吡虫啉、啶虫脒、多菌灵、甲基硫菌灵、嘧霉胺、除虫脲、灭幼脲、辛硫磷、苯醚甲环唑和阿维菌素10种农药残留的分析方法。水果样品用乙腈作为提取溶剂经高速匀浆提取，提取液经LC-NH2固相小柱净化富集，以甲醇、水和乙腈作为梯度洗脱的流动相，采用Shiseido CAPCELL PAK MG ⅡC18色谱柱（250 mm×4.6 mm，5 μm）分离，选择270 nm和245 nm双波长进行目标化合物的检测。结果表明：10种农药在0.05-1.0 mg/kg范围内具有良好的线性关系（0.9834-0.9992），检出限为0.005-0.030 mg/kg，定量限为0.020-0.098 mg/kg。0.05、0.10、0.20 mg/kg添加水平的回收率为69.82-88.95%，86.77-110.61%和89.74-110.62%；相对标准偏差（RSD）为6.52-13.24%，5.21-10.32%和3.56-9.88%。与其他方法相比，具有简便、准确、节约试剂和能耗低等优点，适合水果中10种农药残留的同时测定及定量分析。

HPLC with solid-phase extraction （SPE） and UV double wavelength was presented to analysis of imidacloprid, acetamiprid, carbendazim, thiophanate-methyl, primigravida, diflubenzuron, chlorbenzuron,phoxim, difenoconazole and abamectin pesticide residues in strawberry, peach and apple. Sample preparation involves extraction with acetonitrile, and then purification and enrichment by LC-NH2 solid. Chromatographic analysis was performed on Shiseido CAPCELL PAK MG ⅡC18（250 mm×4.6 mm, 5 μm）HPLC column using methyl alcohol, water and acetonitrile as gradient eluents. Dual wavelength at 270 nm and 245 nm was conducted to detect target compounds. All the ten pesticides ranging from 0.05 mg/kg to 1.0 mg/kg had a good linear relationship （0.9834-0.9992）. And the limits of detection and quantification for the ten pesticides were 0.005-0.030 mg/kg and 0.020-0.098 mg/kg, respectively. The average recoveries obtained from samples spiked with standards at concentrations of 0.05, 0.10 and 0.20 mg/kg were in the range of 69.82-88.95%,86.77-110.61% and 89.74-110.62%, respectively, with relative standard deviations （RSD） of 6.52-13.24%, 5.21-10.32% and 3.56-9.88%, respectively. This method can be applied to determine and quantitative analysis of 10 pesticide residues in fruits, which was more convenient operation, higher sensitivity, higher accuracy and better repeatability than other methods.