Vanderford Brett J, Pearson Rebecca A, Rexing David J, Snyder Shane A
Southern Nevada Water Authority, 243 Lakeshore Road, Boulder City, Nevada 89005, USA.
Anal Chem. 2003 Nov 15;75(22):6265-74. doi: 10.1021/ac034210g.
A method has been developed for the trace analysis of 27 compounds from a diverse group of pharmaceuticals, steroids, pesticides, and personal care products. The method employs solid-phase extraction (SPE) and liquid chromatography/tandem mass spectrometry (LC/MS/MS), using electrospray ionization (ESI) in both positive and negative modes and atmospheric pressure chemical ionization in positive mode. Unlike many previous methods, a single SPE procedure using 1 L of water coupled to a simple LC method is used for all ionization modes. Instrument detection limits for most compounds were below 1.0 pg on column with reporting limits of 1.0 ng/L in water. Recoveries for most compounds in deionized water were greater than 80%. Sulfuric acid was found to be the preferred sample preservative, and structures of all MS/MS product ions are proposed. Matrix effects from waters with a high content of treated municipal effluent were observed in both ESI modes and are discussed in the paper.
已开发出一种用于痕量分析27种化合物的方法，这些化合物来自多种药物、类固醇、农药和个人护理产品。该方法采用固相萃取（SPE）和液相色谱/串联质谱（LC/MS/MS），在正、负离子模式下均使用电喷雾电离（ESI），在正模式下使用大气压化学电离。与许多先前的方法不同，对于所有电离模式，均使用单一的SPE程序（使用1 L水）与简单的LC方法相结合。大多数化合物的仪器检测限在柱上低于1.0 pg，水中报告限为1.0 ng/L。去离子水中大多数化合物的回收率大于80%。发现硫酸是首选的样品防腐剂，并提出了所有MS/MS产物离子的结构。在两种ESI模式下均观察到来自含有高含量经处理城市污水的水样的基质效应，本文对此进行了讨论。
