Determination of oseltamivir phosphate and its metabolite with other pharmaceuticals in surface waters using solid phase extraction and isotope dilution liquid chromatography/tandem mass spectrometry
Determination of oseltamivir phosphate and its metabolite with other pharmaceuticals in surface waters using solid phase extraction and isotope dilution liquid chromatography/tandem mass spectrometry
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固相萃取-同位素稀释液相色谱/串联质谱法测定地表水中磷酸奥司他韦及其代谢物和其他药物
DOI：
10.1080/03067319.2019.1637425
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发表时间：
2020
影响因子：
2.6
通讯作者：
Takashi Kobayashi
中科院分区：
文献类型：
--
作者：
Osamu Kiguchi;Tomoe Ishii;Takuma Watanabe;Rokuro Konno;Akiko Matsubuchi;Takashi Kobayashi
固相萃取和同位素稀释（ID）液相色谱/串联质谱（LC/MS/MS）被用来定量浓度的磷酸奥司他韦及其代谢物（奥司他韦羧酸盐），除了四种药物（咖啡因，卡马西平，三氯生，三氯卡班）在表面沃茨。结果同时有效地阐明了这些化合物在地表沃茨中的发生、归宿和影响。使用含有0.01%甲酸和0.5 mM乙酸铵的超纯水/甲醇梯度作为移动的相，获得目标化合物的更高响应强度。甲醇/乙酸乙酯= 1：4（v/v）有效地将目标化合物从亲油-亲脂平衡的聚合物柱中洗脱。在pH 2.0-3.5下的样品提取不影响回收率。该方法具有良好的线性关系（r ~ 2> 0.9957），并能准确定量。超纯水和河水样品的加标回收率分别为81-127%（RSD为1.2-16%）和89-106%（RSD为0.4- 19%）。超纯水中较低浓度加标水平的方法检测限为0.2-1.9 ng L− 1。该方法应用于日本秋田县一个小流域的样品时，检测到大多数目标化合物的浓度从低到高纳克每升。
Solid phase extraction and isotope dilution (ID) liquid chromatography/tandem mass spectrometry (LC/MS/MS) were used to quantify concentrations of oseltamivir phosphate and its metabolite (oseltamivir carboxylate) in addition to four pharmaceuticals (caffeine, carbamazepine, triclosan, triclocarban) in surface waters. Results simultaneously and effectively elucidate the occurrence, fate, and effects of those compounds in surface waters. Higher response intensities of target compounds were obtained using an ultra-purified water/methanol gradient containing 0.01% formic acid with 0.5 mM ammonium acetate as the mobile phase. Methanol/ethyl acetate = 1:4 (v/v) efficiently eluted target compounds from a hydrophilic–lipophilic balanced polymer cartridge. Sample extraction at pH 2.0–3.5 did not affect recovery. This developed method showed satisfactory linearity (r2> 0.9957) and accurate quantification using ID method with each labelled internal compound. The recoveries from the spiked ultra-purified water and river water samples were 81–127% (1.2–16% relative standard deviation, RSD) and 89–106% (0.4–19%RSD), respectively. The method detection limit was found as 0.2–1.9 ng L−1from spiked levels of lower concentrations in ultra-purified water. This method, when applied to samples from a small river basin in Akita prefecture, Japan, detected most target compounds at low to high nanogram-per-litre concentrations.