气相色谱-三重四级杆串联质谱法测定塑料供水管材中11种邻苯二甲酸酯

Determination of 11 phthalates in plastic pipe for water supply by gas chromatography-triple quadrupole mass spectrometry

目的建立塑料供水管材中11种邻苯二甲酸酯的气相色谱-三重四级杆串联质谱检测方法。方法取250 ml塑料管材浸泡水,经10 ml正己烷萃取3次,萃取液氮气浓缩,用DB-5MS色谱柱(30 m×0.25 mm,0.25μm)分离,由三重四级杆质谱多反应监测(MRM)模式进行定量。结果 11种邻苯二甲酸酯在0.05~1.0 mg/L线性范围内均呈较好的线性关系,r>0.998。检出限为0.008~0.021μg/L,平均回收率为77.5%~92.3%,RSD为3.9%~11.0%。结论该方法快速简便,准确度和精密度均较高,适用于管材中11种邻苯二甲酸酯含量的同时测定。

Objective To establish a method for the determination of 11 phthalates in plastic pipe for water supply by gas chromatography-triple quadrupole mass spectrometry（ GC-MS/MS）. Methods Phthalates in 250 ml soak water of plastic pipe were extracted with 10 ml hexane three times,evaporated by nitrogen and separated by DB-5MS（ 30 m × 0. 25 mm,0. 25 μm）column,then determined by tandem mass spectrometry in multi reaction monitoring mode（ MRM）. Results The regression coefficients（ r） of 11 phthalates were over 0. 998. The calibration curve were linear within the range of 0. 05 ~ 1. 0 mg/L. The limits of detection were 0. 008 ~ 0. 021 μg/L. The average recoveries of 11 phthalates were 77. 5% ~ 92. 3%,and the relative standard deviations were 3. 9% ~ 11. 0%. Conclusion This method is fast,simple,high accuracy and precision and suitable for determining 11 phthalates in plastic pipe for water supply