Lee Hing-Biu, Sarafin Kurtis, Peart Thomas E
Aquatic Ecosystem Protection Research Division, Water Science and Technology Directorate, Science and Technology Branch, Environment Canada, 867 Lakeshore Road, Burlington, Ontario L7R 4A6, Canada.
J Chromatogr A. 2007 May 4;1148(2):158-67. doi: 10.1016/j.chroma.2007.03.024. Epub 2007 Mar 16.
A method using solid-phase extraction (SPE) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been developed for the determination of 12 beta-blockers and beta(2)-agonists in wastewater samples. Extraction of the drugs was effected by an Oasis MCX cartridge with a strong cation resin adsorbent. Matrix coextractives were removed from the SPE cartridge by methanol prior to the elution of the drugs with a mixture of dichloromethane, 2-propranol, and ammonium hydroxide. The extract was analyzed by LC-MS/MS with electrospray ionization operating in the positive mode. Recovery of the 12 compounds was in most cases better than 85% at the fortification levels of 500 and 50 ng/L, with standard deviations between 3 and 7%. Based on a concentration factor of 250, the method detection limits ranged from 6 to 11 ng/L for the target compounds. No degradation of these drugs in spiked sewage effluent samples was observed over a storage period of 7 days at 4 degrees C in the dark. Many beta-blockers were detected in the 14 wastewater samples collected from seven Canadian sewage treatment plants; those occurring at the highest concentrations were atenolol, acebutolol, sotalol, and metroprolol, with overall median concentrations of 1370, 339, 282, and 257 ng/L, respectively. However, there was only a small decrease in the median concentrations of these beta-blockers between the primary and final effluent, suggesting that these drugs are not easily removed by the sewage treatment processes. As a result of selective extraction and effective removal of coextractives, no matrix effect was observed for the samples during LC-MS/MS analyses.
已开发出一种使用固相萃取（SPE）和液相色谱 - 串联质谱（LC - MS/MS）的方法来测定废水样品中的12种β受体阻滞剂和β₂激动剂。药物的萃取通过带有强阳离子树脂吸附剂的Oasis MCX柱进行。在用二氯甲烷、2 - 丙醇和氢氧化铵的混合物洗脱药物之前，先用甲醇从SPE柱上去除基质共萃取物。提取物通过正模式电喷雾电离的LC - MS/MS进行分析。在500和50 ng/L的加标水平下，12种化合物的回收率在大多数情况下优于85%，标准偏差在3%至7%之间。基于250的浓缩因子，目标化合物的方法检测限为6至11 ng/L。在4℃黑暗条件下储存7天期间，未观察到加标污水流出物样品中这些药物的降解。从加拿大七个污水处理厂采集的14个废水样品中检测到许多β受体阻滞剂；浓度最高的是阿替洛尔、醋丁洛尔、索他洛尔和美托洛尔，总体中位浓度分别为1370、339、282和257 ng/L。然而，这些β受体阻滞剂在初级和最终流出物中的中位浓度仅略有下降，这表明这些药物不易通过污水处理过程去除。由于选择性萃取和共萃取物的有效去除，在LC - MS/MS分析过程中未观察到样品的基质效应。
