他莫昔芬和来曲唑常用于治疗雌激素依赖型乳腺癌。本研究建立了城市污水中他莫昔芬和来曲唑的超高效液相色谱-串联质谱(UPLC-MS/MS)联用检测方法。水样通过Oasis HLB固相萃取柱富集后串联氨基柱,先用6 mL甲醇洗脱,再用3 mL甲醇洗脱氨基柱,合并洗脱液后浓缩。使用ACQUITY UPLCTM BEH C18反相柱,流动相为0.1%甲酸-乙腈,在梯度条件下分离;目标分析物使用超高效液相色谱-电喷雾串联质谱进行测定。本方法对他莫昔芬和来曲唑的线性范围分别是1.0~100μg/L和0.1~100μg/L,相关系数R^2〉0.997,检出限分别为1.0和0.1 ng/L,进水和出水的3个不同水平的加标平均回收率为68.8%~103.0%,相对标准偏差小于15%。本方法可用于城市污水中相关物质的分析。
Tamoxifen and letrozole are two of the most effective pharmaceuticals mainly used in hormonal dependent breast cancer therapy.A trace analytical method using ultra performance liquid chromatography/tandem mass spectrometry(UPLC-MS/MS) was developed to simultaneously detect these two drugs in both influent and effluent of municipal sewage treatment plant.Sewage samples were passed through an Oasis HLB cartridge,then an amino solid phase extraction cartridge was connected with Oasis HLB cartridge.Target compounds was firstly eluted with 6 mL methanol and then 3 mL methanol was used to elute the amino solid phase extraction cartridge,collected and pooled the elutants.After concentration,target compounds were separated on a BEH C_18 column using a gradient elution profile with a mobile phase consisting of 0.1% formic acid aqueous solution and acetonitrile and detected by an electro spray ionization tandem mass spectrometry with multiple reactions monitoring(MRM).Satisfactory linearity(R^2〉0.997) was obtained over the range of 1.0-100 μg/L and 0.1-100 μg/L for tamoxifen and letrozole,respectively,with limits of quantification(LOQ) of 1.0 and 0.1 ng/L.Mean recoveries of two target compounds(spiked in sewage samples at three concentration levels) ranged from 68.8% to 103.0%,with relative standard deviations(RSD) less than 15%.This method can be applied for the analysis of target drugs sewage samples.