Hama Jawameer R, Strobel Bjarne W
Department of Plant and Environmental Sciences, University of Copenhagen Thorvaldsensvej 40 1871 Frederiksberg Denmark
RSC Adv. 2019 Sep 25;9(52):30350-30357. doi: 10.1039/c9ra05301h. eCollection 2019 Sep 23.
Pyrrolizidine alkaloids (PAs) are produced in plants as defence compounds against insects. PAs present a serious health risk to humans and livestock; therefore it is necessary to have a validated analytical method to monitor PAs in the environment. The objective of this work is to present an UPLC-MS/MS method for quantification of PAs in environmental samples of both soil and water. A fast, reliable, and sensitive approach is developed to identify and quantify PAs in soil and water. Sample preparation was performed by clean-up and pre-concentration of the samples using MCX solid phase extraction cartridges with full optimization, and then PAs were determined by UPLC coupled with TQ-MS. In the liquid chromatography, most of the parameters were optimized and tested including gradient time, solvents, additives, and pH of the mobile phases and flow rate. In addition, the MS parameters of cone voltage, desolvation temperature, cone flows, and collision energy were optimized. The instrument limit of detection (2-7 μg L) and limit of quantification (5-9 μg L) were determined experimentally, and the method was linearity validated up to 1000 μg L. The method was applied to analyse soil and surface water samples collected in April and May 2018 in Vejle, Borup, and Holte, Denmark. In total, 15 PAs were quantified and reported for the first time in environmental samples, in a range of 3-1349 μg kg in soil and 4-270 μg L in surface water.
吡咯里西啶生物碱（PAs）在植物中作为抵御昆虫的防御化合物产生。PAs对人类和牲畜构成严重的健康风险；因此，有必要建立一种经过验证的分析方法来监测环境中的PAs。这项工作的目的是提出一种超高效液相色谱-串联质谱法（UPLC-MS/MS），用于定量分析土壤和水等环境样品中的PAs。开发了一种快速、可靠且灵敏的方法来鉴定和定量土壤和水中的PAs。使用MCX固相萃取柱对样品进行净化和预浓缩，并进行全面优化，以此进行样品前处理，然后通过超高效液相色谱与三重四极杆质谱联用（UPLC-TQ-MS）测定PAs。在液相色谱中，对包括梯度时间、溶剂、添加剂、流动相的pH值和流速在内的大多数参数进行了优化和测试。此外，还对锥孔电压、去溶剂化温度、锥孔气流和碰撞能量等质谱参数进行了优化。通过实验确定了仪器检测限（2 - 7 μg/L）和定量限（5 - 9 μg/L），该方法在高达1000 μg/L的范围内进行了线性验证。该方法应用于分析2018年4月和5月在丹麦韦勒、博鲁普和霍尔特采集的土壤和地表水样品。总共首次在环境样品中定量分析了15种PAs，土壤中的含量范围为3 - 1349 μg/kg，地表水中的含量范围为4 - 270 μg/L。
