气相色谱-三重四极杆串联质谱法同时测定饮用水中24种邻苯二甲酸酯
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(佛山市南海区疾病预防控制中心,广东 佛山 528200)

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黎少映 女 主管技师 研究方向为理化检验 E-mail:506861459@qq.com

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佛山市南海区“十三五”重点专科(特色专科)建设项目


Determination of 24 phthalate esters in drinking water by gas chromatorgraphy-triple quadrupole mass spectrometry
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(Nanhai Center for Disease Prevention and Control,Guangdong Foshan 528200,China)

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    摘要:

    目的 建立气相色谱-三重四极杆串联质谱同时测定饮用水中24种邻苯二甲酸酯类化合物的方法。方法 250 ml水样过C18玻璃固相萃取柱吸附,6 ml乙酸乙酯洗脱,旋蒸近干,1.0 ml正己烷溶解定容,进样体积为1 μl,HP-5MS色谱柱(30 m×0.25 mm,0.25 μm)分离,采用多反应监测(MRM)模式测定,外标法定量。结果 24种化合物线性关系良好,相关系数(r)均>0.995,方法检出限为0.014~0.50 μg/L,定量限为0.047~1.7 μg/L,平均回收率为80.2%~113.7%,相对标准偏差为2.7%~10.3%(n=6)。应用该方法测定10份不同水质样品,结果共检出9种邻苯二甲酸酯。结论 本方法准确可靠、精密度高、简便快速,适用于同时检测饮用水、水源水和瓶装水中24种邻苯二甲酸酯。

    Abstract:

    Objective To establish a method for the determination of 24 phthalate esters(PAEs)in drinking water by gas chromatorgraphy-triple quadrupole mass spectrometry. Methods PAEs in drinking water were absorbed by C18 glass solid phase extraction(SPE)column and eluted with 6 ml ethyl acetate, rotary evaporated to dry and dissolved in 1 ml N-hexane. The volumn of injection was 1 μl. The sample was separated on a HP-5MS capillary column (30 m×0.25 mm,0.25 μm), and the identification and quantification were performed by gas chromatorgraphy-triple quadrupole mass spectrometry in multiple reaction monitoring (MRM) mode. The external standard method was used for quantification. Results Twenty-four compounds had a good linear relationship (r>0.995).The limits of detection(LODs) were 0.014-0.50 μg/L and the limits of quantification(LOQs) were 0.047-1.7 μg/L. The recoveries at three spiked levels were between 80.2%-113.7%, and the relative standard deviation were between 2.7%-10.3%(n=6). Ten different water samples and nine PAEs were detected by this method. Conclusion This method was accurate, precisive and rapid and it was suitable for simultaneous detection of 24 PAEs in drinking water, source water and bottled water.

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黎少映,冯耀基,吴雪梅,兰红军.气相色谱-三重四极杆串联质谱法同时测定饮用水中24种邻苯二甲酸酯[J].中国食品卫生杂志,2019,31(2):125-131.

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  • 收稿日期:2019-01-31
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  • 在线发布日期: 2019-05-17
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