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多残留方法测定土壤和沉积物中 32 种人用和兽用药物的压力液体萃取和 LC-MS/MS。

Multiresidue method for the determination of 32 human and veterinary pharmaceuticals in soil and sediment by pressurized-liquid extraction and LC-MS/MS.

机构信息

Departamento de Química Física, Facultad de Ciencias del Mar y Ambientales, Universidad de Cádiz, Campus Río San Pedro s/n, 11510, Puerto Real, Cádiz, Spain.

出版信息

Anal Bioanal Chem. 2010 Oct;398(3):1173-84. doi: 10.1007/s00216-010-3862-x. Epub 2010 Jun 19.

Abstract

An analytical chemical method has been developed for the simultaneous determination of 32 different pharmaceuticals in soils and sediments. The pharmaceuticals cover a varity of different compound groups. Soil samples were extracted with different solvents with the help of pressurized-liquid extraction (PLE) followed by clean-up using a solid-phase extraction (SPE) procedure. The purified extracts were analyzed by LC-MS/MS. The extraction method was evaluated by testing the following variables: extraction solvents, solvent pH, and temperature. Applying 20 g of soil/sediment and extracting with a mixture of methanol with aqueous ammonia solution (0.1 mol L(-1)) at 80 degrees C for 5 min in five cycles provided satisfactory recoveries between 66 and 114% with SD of between 1 and 14%. For preconcentration and purification tandem MAX-HLB cartridges were used. The volume and composition was optimized and the highest recoveries were obtained with a combination of methanol-aqueous ammonia solution. The limits of quantification (LOQs) were between 0.2 and 2 ng g(-1) and linearity higher than 0.98 for the majority of the selected pharmaceuticals. The method was successfully applied to soil samples collected from the Jerez de la Frontera agricultural region, irrigated with treated wastewater, and to sediment samples from the River Guadalete. The detection of nine pharmaceuticals including stimulants, antirheumatics, analgesics, anti-inflammatories, tranquilizers, and veterinary medicines at ng g(-1) concentration levels was achieved.

摘要

已经开发出一种分析化学方法,用于同时测定土壤和沉积物中 32 种不同的药物。这些药物涵盖了多种不同的化合物。在加压液体萃取(PLE)的帮助下,使用不同的溶剂提取土壤样品,然后使用固相萃取(SPE)程序进行净化。用 LC-MS/MS 分析纯化提取物。通过测试以下变量来评估提取方法:提取溶剂、溶剂 pH 值和温度。应用 20 克土壤/沉积物,用甲醇与氨水溶液(0.1 mol L(-1))的混合物在 80°C 下提取 5 分钟,进行五次循环,可获得 66%至 114%之间的满意回收率,标准偏差为 1%至 14%。对于预浓缩和净化,串联使用 MAX-HLB 卡。优化了体积和组成,甲醇-氨水溶液的组合可获得最高的回收率。大多数选定药物的定量限(LOQ)在 0.2 和 2 ng g(-1)之间,线性度高于 0.98。该方法成功应用于经处理废水灌溉的赫雷斯德拉弗隆特拉农业区的土壤样品和瓜达莱特河的沉积物样品。在 ng g(-1)浓度水平下检测到九种药物,包括兴奋剂、抗风湿药、镇痛药、消炎药、镇静剂和兽药。

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