新型硅酸镁(1:6)用于几种蔬菜中4-壬基酚净化效果研究

Effects of new magnesium silicate(1∶6)on cleanup of 4-nonylphenol in various vegetables

壬基酚检测需要吸附性能好且成本低的净化材料。通过溶胶-凝胶法制备新型硅酸镁(MS-1:6)材料,考察其吸附性能,作为固相萃取材料用于净化白菜、四季豆、黄瓜、生菜和洋葱5种基质中4-壬基酚,结合液相色谱-串联质谱仪(LC-MS∕MS)测定。结果表明:25℃下新型硅酸镁材料(1:6)对4-NP的最大吸附量为30.84 mg∕g。洗脱液5.0 m L乙腈的条件下对4-NP回收率最高。与商品化吸附材料氨基化多壁碳纳米管(AMCNTs)、多层氧化石墨烯(GO)和N-丙基乙二胺(PSA)相比,MS-1:6对基质效应的降低作用仅次于GO,优于AMCNTs和PSA。具有较高的经济优势,价格仅为GO的1∕1 500。考察MS-1:6循环利用性,结果显示该萃取柱在6次吸附解析循环后,回收率仍在80%以上。平均回收率为88.63%—106.82%,相对标准偏差(RSD)为1.5%—10.86%,检出限为0.6—0.8μg∕kg,定量限为2μg∕kg。该方法简单、快速、成本较低,具有较好的净化效果,能够满足蔬菜中4-壬基酚的检测需要。

The detection of nonylphenol require purification materials with good adsorption performance and low cost.A novel magnesium silicate(MS-1∶6)material was prepared by sol-gel method and its adsorption property was investigated.It was used as a solid-phase extraction material to purify 4-nonylphenol in five matrices including Chinese cabbage,green beans,cucumber,lettuce and onion,and it was determined by liquid chromatography-tandem mass spectrometry(LC-MS∕MS).The results showed that the maximum adsorption capacity of 4-NP on the new magnesium silicate material(1∶6)at 25℃was 30.84 mg∕g.The highest recovery of 4-NP was achieved with 5.0 mL acetonitrile as the eluent.Compared with commercial adsorption materials such as aminated multi-walled carbon nanotubes(AMCNTs),multilayer graphene oxide(GO)and primary secondary amine(PSA)sorbent,the reduction of matrix effect by MS-1∶6 was second to that of GO and was superior to AMCNTs and PSA.Has a high economic advantage,the price is only 1∕1500 of GO.The recycle property of MS-1∶6 was investigated and that result showed that the recovery rate was still above 80%after six adsorption and desorption cycles.The average recovery was 88.63%—106.82%,the relative standard deviation(RSD)was 1.5%—10.86%,and the detection limit was 0.6—0.8μg∕kg,with the quantitation limit of 2μg∕kg.The method is simple,rapid,and low in cost,has a good purification effect,and can meet the detection requirements of 4-nonylphenol in vegetables.