高效液相色谱串联大气压化学电离源质谱(HPLC-APCI-MS)法测定水中三氯生

建立了高效液相色谱串联大气压化学电离源质谱(HPLC-APCI-MS)测定水中三氯生的方法,预处理采用正己烷液液萃取法萃取三氯生,回收率达99.6%;优化的色谱质谱联机分析条件为:检测波长230 nm,流动相乙腈/水(75∶25),离子源APCI源,负离子模式;该分析方法能在5 min内实现对水中三氯生的定性与定量分析.质量保证(Quality Assurance,QA)与质量控制(Quality Control,QC)研究得出,仪器检测限为0.18μg·L-1,相对标准偏差(relative standard deviations,RSD)为0.59%;空白加标实验回收率为103%,RSD为1.2%;以城市生活污水、河水和自来水为加标基质实验回收率为96.6%—108%,方法检测限为0.26—0.61μg·L-1,RSD为0.28%—0.81%.该方法操作简便,分析方法准确性、精密性与可靠性均较高.

Determination of triclosan with HPLC-APCI-MS

In this paper,the method for triclosan determination in water by high performance liquid chromatography and mass spectrometry with atmospheric pressure chemical ionization(HPLC-APCI-MS) was established.Triclosan was extracted from the sample by hexane,then the concentrated extract was determined by HPLC-APCI-MS,and the recovery rate was about 99.6%.The optimum conditions for triclosan determination were as follows.The detection wavelength was 230 nm,the mobile phase was 75/25(V/V) MeCN/H2O and the ion source was APCI(-).Under such conditions,triclosan was separated and determined accurately in 5 minutes.The Quality Asaurance and Quality Control(QA/QC) studies were conducted and the results showed that the instrument detection limits(IDL) of HPLC-MS for triclosan determination was 0.18 μg·L-1,and the relative standard deviations(RSD) was 0.59%.In the spiked blank experiments,the recovery rate reached 103%,and RSD was 1.2%.Moreover,the sanitary sewage,river water and drinking water were used as spiking matrix,the recovery rate was 96.6%—108%,the method detection limits(MDL) was 0.26—0.61 μg·L-1 and RSD was 0.28%—0.81%.The results showed this method had good accuracy,precision and reproducibility.