植物油中4种琥珀酸脱氢酶杀菌剂的测定  

Determination of 4 Succinate Dehydrogenase Inhibitor Fungicides in Vegetable Oils

作　　者：罗本越 LUO Benyue(Xiamen Hongyi Testing Co.,Ltd.,Xiamen 361000)

机构地区：[1]厦门泓益检测有限公司,厦门361000

出　　处：《食品工业》2024年第7期277-281,共5页The Food Industry

摘　　要：建立超高效液相色谱-三重四极杆质谱法(UPLC-MS-MS)快速测定不同植物油中联苯吡菌胺、异丙噻菌胺、氟唑菌酰胺及吡噻菌胺的方法。样品用乙腈提取,经PSA、C_(18)粉末分散固相萃取净化除杂。过0.22μm滤膜后,采用甲醇-0.1%甲酸水为流动相进行梯度洗脱,经C_(18)色谱柱分离, UPLC-MS-MS测定,外标法定量。该方法检出限为0.002 mg/kg,定量限为0.005 mg/kg,在1~200 ng/mL浓度范围时线性系数良好(r>0.99)。在0.005, 0.010和0.020 mg/kg 3个添加水平下,不同植物油基质(大豆油、花生油、玉米油、菜籽油、橄榄油)中4种化合物回收率在78.6%~118.2%之间,相对标准偏差S_(RSD)在0.8%~9.6%之间(n=6)。该方法操作简单、快速、除杂效果好、定量结果准确,适用于植物油中珀酸脱氢酶抑制剂杀菌剂的测定。A method was developed for the fast determination of bixafen,isofetamid,luxapyroxad and penthiopyrad residues in vegetable oils by ultra-high performance liquid chromatography-tandem mass spectrometry(LC-MS/MS)coupled with modified QuEChERS.Samples were extract with acetonitrile,and then the supernatant was purified with primary secondary amine(PSA)and octadecyl trimethoxysilane powder(C_(18)).The 4 compounds were separated on a Cig column by gradient elution using methanol-0.1%(V/V)formic acid in water as the mobile phase after filtered through a 0.22μm membrane,detected by UPLC-MS/MS,and quantified by the external standard method.The limits of detection and limits of quantitation for the method were 0.002 mg/kg and 0.005 mg/kgrespectively.The calibration curves for all analytes showed good linearity in the range of 1-200 ng/mL.The recoveries of the four analytes spiked at three levels(0.005,0.010 and 0.020 mg/kg)in different matrices(soybean oil,peanut oil,corn oil,rapeseed oil,olive oil)ranged from 78.6%to 118.2%with the relative standard deviations(S_(RSD),n=6)from 0.8%-9.6%.The method was easy and fast,and showed good purification efficiency and the results are accurate,which is suitable for the determination of succinate dehydrogenase inhibitor fungicides in vegetableoils.

关 键 词：液相色谱质谱联用仪 植物油 琥珀酸脱氢酶抑制剂杀菌剂 

分 类 号：TS225.1[轻工技术与工程—粮食、油脂及植物蛋白工程]