分散液液微萃取-气相色谱/质谱法测定松茸中18种邻苯二甲酸酯  

Determination of 18 phthalate acid esters in matsutake by dispersive liquid-liquid microextraction-gas chromatography/mass spectrometry

作　　者：王佳敏 邹海民 王希希[2] 薛勇[2] 肖江雨 孙成均 WANG Jia-min;ZOU Hai-min;WANG Xi-xi;XUE Yong;XIAO Jiang-yu;SUN Cheng-jun(West China School of Public Health and West China Fourth Hospital,Chengdu,Sichuan 610041,China)

机构地区：[1]四川大学华西公共卫生学院/华西第四医院,成都610041 [2]成都市疾病预防控制中心,成都610041

出　　处：《现代预防医学》2020年第7期1291-1295,共5页Modern Preventive Medicine

摘　　要：目的建立松茸中18种邻苯二甲酸酯类(PAEs)的分散液液微萃取-气相色谱/质谱分析方法(DLLME-GC/MS),并用于松茸中邻苯二甲酸酯的污染调查。方法样品经乙腈超声提取后,经三氯甲烷分散液液微萃取,氮吹干、甲醇复溶后进样测定,内标法定量。结果方法线性范围为0.001~1.00 mg/L(DBEP和DCHP为0.005~1.00 mg/L),相关系数均大于0.9995。方法检出限为0.10~0.85μg/kg,定量限为0.33~2.84μg/kg。在3个加标浓度水平下的加标回收率为80.23%~118.0%,相对标准偏差为1.38%~14.7%。用本法检测了18个松茸样品,检出多种PAEs,总含量范围(∑PAEs)为12.62~5430μg/kg。结论该方法具有简单、快速、灵敏、价廉等优点,适用于松茸中18种邻苯二甲酸酯的测定。Objective To establish a method for the determination of 18 phthalate acid esters(PAEs)in matsutake by dispersive liquid-liquid microextraction-gas chromatography-mass spectrometry(DLLME-GC/MS),and to investigate the contamination status of PAEs in matsutakes.Methods PAEs in samples were extracted by ultrasound with acetonitrile,and then liquid-liquid microextracted with trichloromethane which was taken and dried-up under nitrogen gas,finally the residue was dissolved with methanol,and the solution was injected to GC/MS for analysis.The quantification was based on the internal standard curves.Results The linear ranges of the method were 0.001-1.00 mg/L(DBEP and DCHP were 0.005-1.00 mg/L),with the correlation coefficients all greater than 0.9995.The limits of detection(LODs)was 0.10-0.85μg/kg and the limits of quantification(LOQs)was 0.33-2.84μg/kg.The recoveries were 80.23%-118.0%and the relative standard deviations(RSDs)were 1.38%-14.69%.Some of PAEs were detected in 18 matsutake samples by this method and the total contents of PAEs ranged from 12.62 to 5430 g/kg.Conclusion The method is simple,rapid,sensitive and cheap.And it is suitable for simultaneous determination of 18 PAEs in matsutake.

关 键 词：邻苯二甲酸酯 松茸 分散液液微萃取 气相色谱-质谱法 

分 类 号：R446.12[医药卫生—诊断学]