Department of Chemistry, University at Buffalo, The State University of New York, Buffalo, New York 14260, United States.
J Agric Food Chem. 2011 Mar 23;59(6):2213-22. doi: 10.1021/jf104355x. Epub 2011 Feb 22.
The ability to monitor multiple analytes from various classes of compounds in a single analysis can increase throughput and reduce cost when compared to traditional methods of analyses. This method for analyzing free (parent estrogen) and conjugated estrogens (metabolites) along with sulfonamides and tetracyclines utilizes a high pH (10.4) mobile phase with an ammonium hydroxide buffer for both positive- and negative-mode electrospray ionization. A single-step sample preparation by solid-phase extraction (SPE) was used to isolate and concentrate all analytes simultaneously. The analytical method was developed and validated for recoveries at 3 concentration levels for water and soil and produced recoveries of 42-123% and 21-105% respectively. Method detection limits ranged from 0.3 to 1.0 ng/L for water samples and 0.01 to 0.1 ng/g for soils. The method quantification limit ranged from 0.9 to 3.3 ng/L for water samples and 0.06 to 0.7 ng/g for soils. The single-point standard addition calibration procedure was validated across a linear range of MQL to 100 ng/L with ≥82% accuracy against a matrix matched standard curve. Furthermore, sorption of tetracyclines onto glassware was investigated and minimized by 10% using nitric acid-rinsed glassware, while separation parameters were further optimized based on retention time and signal responses. This method has been used for the quantification of estrogens, tetracyclines, and sulfonamides in soil and runoff waters with multiple compounds detected simultaneously in a single analysis.
与传统分析方法相比，能够在单次分析中监测来自各种化合物类别的多种分析物，可提高通量并降低成本。这种用于分析游离（母体雌激素）和结合雌激素（代谢物）以及磺胺类药物和四环素类药物的方法，使用高 pH 值（10.4）的流动相和氨缓冲液进行正离子和负离子电喷雾电离。通过固相萃取 (SPE) 进行单步样品制备，同时分离和浓缩所有分析物。该分析方法是为水和土壤中的 3 个浓度水平的回收率而开发和验证的，回收率分别为 42-123%和 21-105%。方法检测限范围为水样品 0.3-1.0ng/L 和土壤 0.01-0.1ng/g。方法定量限范围为水样品 0.9-3.3ng/L 和土壤 0.06-0.7ng/g。单点标准添加校准程序在 MQL 到 100ng/L 的线性范围内进行了验证，与基质匹配标准曲线相比，准确度≥82%。此外，通过使用硝酸冲洗的玻璃器皿，研究并将四环素类药物对玻璃器皿的吸附减少了 10%，同时还根据保留时间和信号响应进一步优化了分离参数。该方法已用于土壤和径流水中雌激素、四环素类药物和磺胺类药物的定量分析，可在单次分析中同时检测多种化合物。
