超高效液相色谱-大气压化学电离-串联质谱法测定生活饮用水中痕量苯并(a)芘

Determination of trace benzo(a)pyrene in drinking water by ultra performance liquid chromatography-atmospheric pressure chemical ionization-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  大气压化学电离模式  生活饮用水  苯并(a)芘

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  atmospheric pressure chemical ionization mode  drinking water  benzo(a)pyrene

中文摘要:

      目的 建立超高效液相色谱-大气压化学电离-串联质谱法(ultra performance liquid chromatography-atmospheric pressure chemical ionization-tandem mass spectrometry, UPLC-APCI-MS/MS)测定水中痕量苯并(a)芘的检测方法。方法 样品前处理用环己烷洗脱的固相萃取法, 以乙腈-水为流动相进行梯度洗脱, 流速为0.6 mL/min, 进样量为10 μL, 使用HPLC column Shim-pack GIST C18色谱柱分离, 在正离子APCI多反应监测模式进行测定。结果 在优化后的条件下进行方法学验证, 苯并(a)芘在质量浓度为0.50~70.00 μg/L的范围内有良好的线性关系, r2为0.9992, 检出限为0.484 ng/L, 定量限为1.940 ng/L, 分别对生活饮用水、地表水和地下水进行了3个不同水平加标, 平均加标回收率在86.9%~93.5%, 相对标准偏差在0.5%~4.9%。结论 该方法易于操作、检测高效、数据精准、灵敏度高, 适用于生活饮用水及水源水中痕量苯并(a)芘的测定。

英文摘要:

      Objective To establish a method for the determination of trace benzo(a)pyrene in water by ultra performance liquid chromatography-atmospheric pressure chemical ionization-tandem mass spectrometry (UPLC-APCI-MS/MS). Methods Sample pretreatment was performed using solid-phase extraction with cyclohexane as the elution solvent. Gradient elution was carried out with acetonitrile-water as the mobile phase at a flow rate of 0.6 mL/min, and an injection volume of 10 μL. Separation was achieved on an HPLC column Shim-pack GIST C18. Detection was performed in positive ion mode by APCI with multiple reaction monitoring. Results Methodological validation was conducted under optimized conditions, demonstrating a good linear relationship for benz(a)pyrene within the mass concentration range of 0.50–70.0 μg/L (r2=0.9992). The limit of detection was 0.484 ng/L and a limit of quantitation was 1.940 ng/L. The 3 different levels of spiked samples were applied to drinking water, surface water and groundwater, respectively, yielding an average spiked recovery rate of 86.9%–93.5% with relative standard deviations ranging from 0.5% to 4.9%. Conclusion This method is easy to operate, highly efficient in detection, accurate in data and exhibits high sensitivity, making it suitable for the determination of trace benz(a)pyrene in drinking water and source water.