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Development and validation of a UHPLC-MS/MS method for the identification of irinotecan photodegradation products in water samples.
Environmental Pollution ( IF 7.6 ) Pub Date : 2019-10-10 , DOI: 10.1016/j.envpol.2019.113370 Fabio Gosetti 1 , Masho Hilawie Belay 1 , Emilio Marengo 1 , Elisa Robotti 1
Environmental Pollution ( IF 7.6 ) Pub Date : 2019-10-10 , DOI: 10.1016/j.envpol.2019.113370 Fabio Gosetti 1 , Masho Hilawie Belay 1 , Emilio Marengo 1 , Elisa Robotti 1
Affiliation
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Irinotecan (CPT-11) is a water-soluble anticancer drug widely used to treat several types of cancer. Even if the metabolites of CPT-11 are well-known and investigated, only limited information is available in the literature about the formation of photo-degradation products that can naturally originate from sunlight irradiation when the drug is released in aqueous systems. CTP-11 solutions at 10.0 mg L-1 were irradiated by simulated sunlight. The intensity of the drug decreased by 90% after 7.5 days of irradiation and no significant reduction of absorbance values was observed after 13 days. A sensitive UHPLC-MS/MS method was developed employing a hybrid triple quadrupole/linear ion trap mass spectrometer, that is able to work in data-dependent acquisition mode and to obtain information about the compounds formed during the photoirradiation. Moreover, a selected reaction monitoring method was built using the MS/MS fragmentation pattern of the compounds previously investigated. The method was validated considering LOD, LOQ, linearity, precision, selectivity, recovery and matrix effect. LOD and LOQ values were 0.02 and 0.05 ng mL-1, respectively, whereas MDL and MQL values in real water samples (river water, groundwater, well water, and wastewater) were lower than 0.05 and 0.2 ng mL-1, respectively. Eight photodegradation products were identified, among which five for the first time. Based on the MS and MS/MS fragmentation, the chemical structures of the degradation products were proposed. Hydrolysis experiments were carried out on the same solutions preserved in the dark, but no formation of other species was highlighted. The method was applied to several real samples: CPT-11 was detected and quantified only in a hospital effluent sample at the concentration of 0.41 ± 0.2 ng mL-1 together with the occurrence of PDP3. The outcomes of this study may be useful for updating the pollutant screening in water samples.
中文翻译：
开发和验证用于鉴定水样品中伊立替康光降解产物的UHPLC-MS / MS方法。
伊立替康（CPT-11）是一种水溶性抗癌药，广泛用于治疗多种类型的癌症。即使CPT-11的代谢物是众所周知的并已进行了研究，但在文献中仅可获得有限的信息，这些信息涉及光降解产物的形成，当药物在水性体系中释放时，光降解产物自然可以来自阳光照射。用模拟阳光照射10.0 mg L-1的CTP-11溶液。照射7.5天后，药物强度降低了90％，而在13天后未观察到吸光度值显着降低。使用混合三重四极杆/线性离子阱质谱仪开发了一种灵敏的UHPLC-MS / MS方法，该方法能够以数据依赖的采集模式工作，并获得有关光照射过程中形成的化合物的信息。此外，使用先前研究的化合物的MS / MS片段化模式建立了选择的反应监测方法。通过考虑LOD，LOQ，线性，精度，选择性，回收率和基质效应对方法进行了验证。LOD和LOQ值分别为0.02和0.05 ng mL-1，而真实水样（河流水，地下水，井水和废水）中的MDL和MQL值分别低于0.05和0.2 ng mL-1。鉴定出八种光降解产物，其中第一次是五种。基于MS和MS / MS裂解，提出了降解产物的化学结构。水解实验是在黑暗中保存的相同溶液上进行的，但未突出显示其他物种的形成。该方法已应用于几个真实样本：仅在医院污水样品中以0.41±0.2 ng mL-1的浓度检测到CPT-11并对其进行定量，并伴有PDP3的出现。这项研究的结果可能对更新水样中的污染物筛查有用。
更新日期：2019-10-10
中文翻译：
开发和验证用于鉴定水样品中伊立替康光降解产物的UHPLC-MS / MS方法。
伊立替康（CPT-11）是一种水溶性抗癌药，广泛用于治疗多种类型的癌症。即使CPT-11的代谢物是众所周知的并已进行了研究，但在文献中仅可获得有限的信息，这些信息涉及光降解产物的形成，当药物在水性体系中释放时，光降解产物自然可以来自阳光照射。用模拟阳光照射10.0 mg L-1的CTP-11溶液。照射7.5天后，药物强度降低了90％，而在13天后未观察到吸光度值显着降低。使用混合三重四极杆/线性离子阱质谱仪开发了一种灵敏的UHPLC-MS / MS方法，该方法能够以数据依赖的采集模式工作，并获得有关光照射过程中形成的化合物的信息。此外，使用先前研究的化合物的MS / MS片段化模式建立了选择的反应监测方法。通过考虑LOD，LOQ，线性，精度，选择性，回收率和基质效应对方法进行了验证。LOD和LOQ值分别为0.02和0.05 ng mL-1，而真实水样（河流水，地下水，井水和废水）中的MDL和MQL值分别低于0.05和0.2 ng mL-1。鉴定出八种光降解产物，其中第一次是五种。基于MS和MS / MS裂解，提出了降解产物的化学结构。水解实验是在黑暗中保存的相同溶液上进行的，但未突出显示其他物种的形成。该方法已应用于几个真实样本：仅在医院污水样品中以0.41±0.2 ng mL-1的浓度检测到CPT-11并对其进行定量，并伴有PDP3的出现。这项研究的结果可能对更新水样中的污染物筛查有用。
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