García M D Gil, Culzoni M J, De Zan M M, Valverde R Santiago, Galera M Martínez, Goicoechea H C
Departamento de Hidrogeología y Química Analítica, Facultad de Ciencias Experimentales, Universidad de Almería, La Cañada de San Urbano, 04120 Almería, Spain.
J Chromatogr A. 2008 Feb 1;1179(2):115-24. doi: 10.1016/j.chroma.2007.11.049. Epub 2007 Nov 22.
A new powerful algorithm (unfolded-partial least squares followed by residual bilinearization (U-PLS/RBL)) was applied for first time on second-order liquid chromatography with diode array detection (LC-DAD) data and compared with a well-known established method (multivariate curve resolution-alternating least squares (MCR-ALS)) for the simultaneous determination of eight tetracyclines (tetracycline, oxytetracycline, meclocycline, minocycline, metacycline, chlortetracycline, demeclocycline and doxycycline) in wastewaters. Tetracyclines were pre-concentrated using Oasis Max C18 cartridges and then separated on a Thermo Aquasil C18 (150 mm x 4.6mm, 5 microm) column. The whole method was validated using Milli-Q water samples and both univariate and multivariate analytical figures of merit were obtained. Additionally, two data pre-treatment were applied (baseline correction and piecewise direct standardization), which allowed to correct the effect of breakthrough and to reduce the total interferences retained after pre-concentration of wastewaters. The results showed that the eight tetracycline antibiotics can be successfully determined in wastewaters, the drawbacks due to matrix interferences being adequately handled and overcome by using U-PSL/RBL.
一种新的强大算法（展开-偏最小二乘法后接残差双线性化，即U-PLS/RBL）首次应用于二极管阵列检测的二阶液相色谱（LC-DAD）数据，并与一种著名的既定方法（多元曲线分辨-交替最小二乘法，即MCR-ALS）进行比较，用于同时测定废水中的八种四环素（四环素、土霉素、甲氯环素、米诺环素、美他环素、金霉素、地美环素和多西环素）。使用Oasis Max C18柱对四环素进行预富集，然后在Thermo Aquasil C18（150 mm×4.6mm，5微米）柱上进行分离。使用超纯水样品对整个方法进行了验证，并获得了单变量和多变量分析的品质因数。此外，还应用了两种数据预处理方法（基线校正和分段直接标准化），这可以校正穿透效应，并减少废水预富集后保留的总干扰。结果表明，使用U-PSL/RBL可以成功测定废水中的八种四环素抗生素，基质干扰带来的缺点得到了充分处理和克服。
