Lu Lu, Hashi Yuki, Wang Zhi-Hua, Ma Yuan, Lin Jin-Ming
State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, Beijing 100029, China.
Department of Chemistry, Tsinghua University, Beijing 100084, China.
J Pharm Anal. 2011 May;1(2):92-99. doi: 10.1016/S2095-1779(11)70016-8. Epub 2012 Jan 30.
Monolithic silica spin column extraction (MonoSpin-SPE) was developed as a simple, sensitive, and eco-friendly pretreatment method which combined with ultra-fast liquid chromatography-mass spectrometry (UFLC-MS) to determine the levels of six phthalate esters, dimethyl-(DMP), diethyl-(DEP), dipropyl- [DPrP], butyl-benzyl-(BBP), dicyclohexyl(DcHP), and di- phthalate in physiological saline samples. Under optimized experimental conditions, the method was linear in the following ranges: 0.2- 50 μ/L for DMP, DEP, DPrP, DcHP and DOP; 5 - 100 μ/L for BBP. The correlation coefficients (R) were in the range of O. 9951 - O. 9995 for all the analytes and the limits of detection (LODs) and limits of quantification (LOQs) were in the ranges of 0.02 - 0.9 μ/L and 0.08 - 2.7 μ/L, respectively. The pretreatment process showed good reproducibility with inter-day and intra-day relative standard deviations (RSDs) below 8.5% and 11.2%, respectively. This method was used to determine the levels of six phthalate esters in physiological saline samples and the recoveries ranged from 71.2% to 107. 3%. DMP and DEP were found in actual physical saline samples (brand A and brand B).
整体硅胶旋转柱萃取法（MonoSpin-SPE）是一种简单、灵敏且环保的预处理方法，它与超快速液相色谱-质谱联用仪（UFLC-MS）相结合，用于测定生理盐水样品中六种邻苯二甲酸酯的含量，即邻苯二甲酸二甲酯（DMP）、邻苯二甲酸二乙酯（DEP）、邻苯二甲酸二丙酯[DPrP]、邻苯二甲酸丁苄酯（BBP）、邻苯二甲酸二环己酯（DcHP）和邻苯二甲酸二辛酯（DOP）。在优化的实验条件下，该方法在以下浓度范围内呈线性：DMP、DEP、DPrP、DcHP和DOP为0.2 - 50 μ/L；BBP为5 - 100 μ/L。所有分析物的相关系数（R）在0.9951 - 0.9995范围内，检测限（LOD）和定量限（LOQ）分别在0.02 - 0.9 μ/L和0.08 - 2.7 μ/L范围内。预处理过程具有良好的重现性，日间和日内相对标准偏差（RSD）分别低于8.5%和11.2%。该方法用于测定生理盐水样品中六种邻苯二甲酸酯的含量，回收率在71.2%至107.3%之间。在实际的生理盐水样品（A品牌和B品牌）中检测到了DMP和DEP。
