PDF(Pubmed)
Abstract：
Over recent decades, steroidal estrogens have become an emerging and very serious issue as they pose a serious threat to living organisms, soil, plants, and water resources in general. Estrogens have therefore been the subject of considerable scientific attention in order to develop new methodologies for its determination, being able of detecting them at very low concentrations. Those procedures minimize or eliminate the consumption of organic solvents and reagents that may be incompatible with the environment. In this respect, we developed a sensitive, selective method for the simultaneous determination of thirteen natural and synthetic hormones present at the nanogram-per-liter level in various types of water by using continuous solid-phase extraction in combination with gas chromatography and mass spectrometry (GC-MS). The target analytes were preferentially sorbed on an Oasis HLB sorbent column (80 mg) and eluted with acetone (600 µL) for derivatization with a mixture of 70 µL of N,O-bis(trimethylsilyl) trifluoroacetamide and trimethylchlorosilane and 35 µL of petroleum ether in a household microwave oven at 200 W for 4 min. Under optimum conditions, the ensuing method exhibited good linearity (r ≥ 0.998), good precision (RSD ≤ 7%), high recoveries (92-103%), and low detection limits (0.01-0.3 ng L-1). The method outperforms existing alternatives in robustness, sensitivity, throughput, flexibility-it allows both estrogens, progestogens, and androgens to be determined simultaneously-and compliance with the principles of Green Chemistry. It was successfully used to analyze various types of water samples (mineral, tap, well, pond, swimming pool, river, and waste) that were found to contain four estrogens (estrone, 17β-estradiol, 17α-ethinylestradiol, and hexestrol), two progestogens (testosterone, dihydrotestosterone), and one progestogen (progesterone) at concentrations ranging from 3.0 to 110 ng L-1.
摘要：
近几十年来,类固醇雌激素已经成为一个新兴的非常严重的问题，因为它们对生物体构成严重威胁，土壤,植物,和一般的水资源。因此，雌激素一直是相当科学关注的主题，以便开发新的测定方法，能够在非常低的浓度下检测到它们。这些程序最小化或消除了可能与环境不相容的有机溶剂和试剂的消耗。在这方面,我们开发了一种敏感的，通过使用连续固相萃取结合气相色谱和质谱（GC-MS），同时测定各种类型水中纳克/升水平的13种天然和合成激素的选择性方法。目标分析物优先吸附在OasisHLB吸附柱（80mg）上，并用丙酮（600µL）洗脱，以衍生化70µLN的混合物，O-双（三甲基甲硅烷基）三氟乙酰胺和三甲基氯硅烷和35µL石油醚在家用微波炉中以200W持续4分钟。在最佳条件下，随后的方法表现出良好的线性(r≥0.998)，良好的精度（RSD≤7%），高回收率(92-103%)，和低检测限（0.01-0.3ngL-1）。该方法在鲁棒性上优于现有的替代方案，灵敏度,吞吐量，灵活性-它允许两种雌激素，孕激素,和雄激素要同时测定，并符合绿色化学的原则。它被成功地用于分析各种类型的水样(矿物，tap,嗯,池塘,游泳池,河,和废物)被发现含有四种雌激素(雌酮，17β-雌二醇，17α-炔雌醇，和hexestrol)，两种孕激素（睾酮，双氢睾酮)，和一种孕激素（孕酮），浓度范围为3.0至110ngL-1。
