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目的建立全自动固相萃取技术、气相色谱-质谱法测定水源水中22种半挥发有机物的分析方法。方法水样中的被测物经C18固相萃取小柱富集,二氯甲烷和乙酸乙酯洗脱,用气相色谱-质谱法检测,以保留时间和选择离子定性,菲-D10作为内标物定量。结果 22种化合物在试验范围内分离效果好,曲线相关系数>0.996,检出限(LOD)为0.040~0.86μg/L,样品平均加标回收率在89.6%~106.8%,相对标准偏差(RSD)1.45%~6.72%。结论该方法简便、快速,具有较高的准确度与精密度,回收率高,适合于水中半挥发有机物的测定。
OBJECTIVE To establish an analytical method for the determination of 22 semi-volatile organic compounds in drinking water by gas chromatography-mass spectrometry with automatic solid-phase extraction. Methods The analytes in the water sample were enriched with C18 solid phase extraction cartridge, eluted with dichloromethane and ethyl acetate, detected by gas chromatography-mass spectrometry, characterized by retention time and selected ion, phenanthrene-D10 as internal standard Quantitative. Results The results showed that the 22 compounds had good separation performance within the experimental range with a correlation coefficient> 0.996, a limit of detection (LOD) of 0.040-0.86 μg / L and a mean recovery of 89.6% -106.8%. The relative standard deviations (RSDs) ) 1.45% ~ 6.72%. Conclusion The method is simple, rapid, high accuracy and precision, high recovery rate, suitable for the determination of semi-volatile organic compounds in water.