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首页> 外文期刊>Journal of mass spectrometry: JMS >Comparison of multiple API techniques for the simultaneous detection of microconstituents in water by on-line SPE-LC-MS/MS
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Comparison of multiple API techniques for the simultaneous detection of microconstituents in water by on-line SPE-LC-MS/MS

机译：在线SPE-LC-MS / MS同时检测水中微量成分的多种API技术的比较

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This study described a fully automated method using on-line solid phase extraction of large volume injections coupled with high performance liquid chromatography (HPLC) and tandem mass spectrometry (MS/MS) to simultaneously detect a group of recalcitrant microconstituents (pharmaceuticals and personal care products, steroid hormones and sterols) in aqueous matrices. Samples (1 mL to 20 mL) were loaded to the preconcentration column at 1 mL/min, and the column was washed with 1000 μL of 25% methanol in LC/MS water to remove polar and ionic interferences before LC-MS/MS analysis. Three different atmospheric pressure ionization (API) techniques, including photoionization (APPI) with four different dopants (acetone, anisole, chlorobenzene and toluene), heated electrospray ionization (HESI) and atmospheric pressure chemical ionization (APCI), were evaluated on the basis of method detection limits (MDLs) and recoveries from different aqueous matrixes. Results indicated that APPI with toluene as dopant was the most sensitive ionization method for the majority of the analytes. When using 5 mL of sample, MDLs for pharmaceuticals and personal care products, including carbamazepine, DEET, caffeine, naproxen, acetaminophen and primidone, were between 0.3 ng/L and 15 ng/L. MDLs of hormones, including testosterone, equilenin, progesterone, equilin, 17β-estradiol, 17α-ethynylestradiol, estrone, androsterone, mestranol and estriol, were between 1.2 ng/L and 37 ng/L. The combination of APPI with dopant allowed the detection of two difficult to ionize fecal related sterols, such as coprostan-3-ol and coprostan-3-one with MDLs of 5.4 ng/L and 11 ng/L, respectively. Calculated MDLs are more than adequate for analysis of wastewater using 1 to 5 mL sample size and for surface waters using up to 20 mL sample size.
机译：这项研究描述了一种全自动方法，该方法使用大体积进样的在线固相萃取结合高效液相色谱（HPLC）和串联质谱（MS / MS）来同时检测一组顽固的微量成分（药品和个人护理产品） ，类固醇激素和固醇）在水性基质中。以1 mL / min的速度将样品（1 mL至20 mL）上样至预浓缩柱，并在LC-MS / MS分析之前，用1000μL25％的LC / MS水中的甲醇洗涤该柱以去除极性和离子干扰。在以下基础上，评估了三种不同的大气压电离（API）技术：包括使用四种不同的掺杂剂（丙酮，苯甲醚，氯苯和甲苯）的光电离（APPI），加热的电喷雾电离（HESI）和大气压化学电离（APCI）。方法检测限（MDL）和从不同含水基质中的回收率结果表明，对于大多数分析物，以甲苯为掺杂剂的APPI是最灵敏的电离方法。当使用5 mL样品时，包括卡马西平，DEET，咖啡因，萘普生，对乙酰氨基酚和primidone在内的药品和个人护理产品的MDL在0.3 ng / L至15 ng / L之间。激素的MDL值在1.2 ng / L至37 ng / L之间，包括睾丸激素，马来宁，孕酮，马匹林，17β-雌二醇，17α-乙炔基雌二醇，雌酮，雄甾酮，甲雌醇和雌三醇。 APPI与掺杂剂的组合允许检测两种难于电离的粪便相关固醇，例如coprostan-3-ol和coprostan-3-one，其MDL分别为5.4 ng / L和11 ng / L。计算得出的MDL足以用于使用1至5 mL样品量的废水分析和用于最高20 mL样品量的地表水。

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