Lehotay S J, Valverde-García A
US Department of Agriculture, Agricultural Research Service, Beltsville Agricultural Research Center, MD 20705, USA.
J Chromatogr A. 1997 Mar 21;765(1):69-84. doi: 10.1016/s0021-9673(96)00846-1.
This study was designed to determine which combination of sorbent-trap and elution solvent provided the most efficient automated method of collection in supercritical fluid extraction (SFE), elution of analytes, and clean-up of orange, sweet potato and green bean extracts for analysis of 56 diverse pesticides using GC-ion-trap MS. The solid-phase traps evaluated consisted of octyldecylsilane (ODS), diol, Tenax and Porapak-Q, and the elution solvents compared were acetone, ethyl acetate, acetonitrile and methanol. SFE collection by bubbling into each organic solvent was also compared. Recoveries, elution volumes, limits of detection and clean-up aspects were determined for each combination of commodity, trap and solvent tested. High trapping efficiencies were achieved in each case, and acetone usually eluted the pesticides in the least volume (< 1 ml) from the traps. The few matrix components that interfered in GC-ion-trap MS continued to interfere in all trap/solvent pairs, and limits of detection were independent of trap/solvent combination. The use of the ODS trap and acetone elution solvent gave the most consistently high recoveries of the traps and solvents tested.
本研究旨在确定在超临界流体萃取(SFE)中,哪种吸附剂捕集阱和洗脱溶剂的组合能提供最有效的自动化方法,用于收集、分析物洗脱以及净化橙子、红薯和绿豆提取物,以便使用气相色谱 - 离子阱质谱法分析56种不同的农药。所评估的固相捕集阱包括十八烷基硅烷(ODS)、二醇、Tenax和Porapak - Q,所比较的洗脱溶剂为丙酮、乙酸乙酯、乙腈和甲醇。还比较了通过鼓泡进入每种有机溶剂进行SFE收集的情况。针对测试的每种商品、捕集阱和溶剂组合,测定了回收率、洗脱体积、检测限和净化情况。在每种情况下都实现了高捕集效率,并且丙酮通常以最少的体积(<1毫升)从捕集阱中洗脱农药。在气相色谱 - 离子阱质谱中产生干扰的少数基质成分在所有捕集阱/溶剂对中均持续产生干扰,并且检测限与捕集阱/溶剂组合无关。在所测试的捕集阱和溶剂中,使用ODS捕集阱和丙酮洗脱溶剂能获得最稳定的高回收率。