气相色谱-质谱法同时测定水性涂料中3种生物杀伤剂的含量  

Simultaneously Determination of 3 Biocides in Waterborne Coating by Gas Chromatography-Mass Spectrometry

作　　者：蒋莹[1] 诸鸿未[1] 赵霞[1] JIANG Ying;ZHU Hongwei;ZHAO Xia(Shanghai Institute of Quality Inspection and Technical Research,Shanghai 201114,China)

机构地区：[1]上海市质量监督检验技术研究院,上海201114

出　　处：《理化检验（化学分册）》2023年第1期61-64,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：上海市科学技术委员会研发公共服务平台建设项目(14DZ2293000);上海市质量监督检验技术研究院科研项目(KY-2019^(-1)1-QH)。

摘　　要：提出了气相色谱-质谱法同时测定水性涂料中碘代丙炔基氨基甲酸丁酯、百菌清、三氯生等3种生物杀伤剂含量的方法。称取水性涂料样品1 g,加入1 000 mg·L^(-1)正二十烷(内标)溶液500μL,再用乙酸乙酯稀释至10 mL,混匀,超声提取30 min,冷却,以4 000 r·min^(-1)转速离心20 min,取上清液待测。各目标化合物在HP-5ms石英毛细管柱上以柱升温程序分离后,用质谱仪进行检测,内标法定量。结果显示:3种目标化合物标准曲线的线性范围均为0.1~100 mg·L^(-1),检出限(3S/N)为0.033~0.098 mg·kg^(-1);对阴性样品进行3个浓度水平的加标回收试验,回收率为87.1%~103%,测定值的相对标准偏差(n=7)均小于5.0%;方法用于10种实际样品分析,百菌清和三氯生均未检出,1种样品中检出碘代丙炔基氨基甲酸丁酯,检出量为760.7 mg·kg^(-1)。A method for the determination of 3 biocides, including iodopropynyl butylcarbamate, chlorothalonil and triclosan, in waterborne coating by gas ghromatography-mass spectrometry was proposed. The waterborne coating sample(1 g) was taken, and 500 μL of 1 000 mg·L^(-1)n-eicosane(internal standard) solution was added. The mixture was diluted to 10 mL with ethyl acetate, mixed well, and extracted by ultrasound for 30 min. After cooling, the above solution was centrifuged for 20 min at 4 000 r·min^(-1), and the supernatant was taken for determination. The target compounds were separated on HP-5ms quartz capillary column by column heating procedure, detected by mass spectrometer, and quantified by internal standard method. It was shown that the linear ranges of the standard curves of 3 target compounds were 0.1^(-1)00 mg·L^(-1), with detection limits(3S/N) in the range of 0.033-0.098 mg·kg^(-1). Test for recovery was made on the negative sample at 3 conecntration levels, giving results in the range of 87.1%^(-1)03%, and RSDs(n=7) of the determined values were less than 5.0%. This method was applied to analysis of 10 actual samples. Chlorothalonil and triclosan were not detected, and iodopropynyl butylcarbamate was detected in one sample, with detected amount of 760.7 mg·kg^(-1).

关 键 词：气相色谱-质谱法 水性涂料 碘代丙炔基氨基甲酸丁酯 百菌清 三氯生 

分 类 号：O652.63[理学—分析化学]