超高效液相色谱-电喷雾质谱法结合同位素稀释技术检测动物源性食品中的六溴环十二烷异构体  

Analysis of hexabromocyclododecane diastereoisomers in foods of animal origin using ultra performance liquid chromatography-mass spectrometry and isotope dilution

作　　者：施致雄[1,2] 封锦芳[2] 李敬光[1] 赵云峰[1] 吴永宁[1,2] 

机构地区：[1]中国疾病预防控制中心营养与食品安全所,北京100050 [2]首都医科大学公共卫生与家庭医学学院,北京100069

出　　处：《色谱》2008年第1期1-5,共5页Chinese Journal of Chromatography

基　　金：国家高技术研究发展计划(“863”计划)专题课题(No.2006AA06Z043);“十一五”国家科技支撑计划重大项目(No.2006BAK02A10);北京市教育委员会科技发展计划项目(No.KM200810025022).

摘　　要：建立了使用超高效液相色谱-电喷雾四极杆质谱（UPLC-ESI-MS）结合同位素稀释技术准确测定动物源性食品中六溴环十二烷（HBCD）的3种非对映异构体的方法。试样在加入同位素内标13^C-HBCD后进行索氏提取,提取液去除脂肪后经硅胶固相萃取柱浓缩、净化后,通过Waters ACQUITY UPLCTMBEH C18色谱柱分离,以甲醇-乙腈混合液和水为流动相进行梯度洗脱。在UPLC-MS分析过程中以保留时间和母离子信息进行定性,选择离子记录（SIR）方式定量。该法对于所测试的鲜奶、鱼肉等样品,检出限为0.1-0.4ng/g,定量限为0.4-1.2ng/g。对于加标鱼肉样品,添加水平为0.6,2.0和6.0ng/g时,3种被测物的加标回收率为92.9%-99.3%,相对标准偏差为3.1%-8.0%。A method for the detection of the α, βand γ-diastereoisomers of hexabromocyclododecane （HBCDs） in foods of animal origin, such as fish, chick, milk, butter etc. , was developed using ultra performance liquid chromatography-electrospray ionization mass spectrometry （UPLC-ESI-MS） and isotope dilution. The HBCDs with the spiked isotopic 13^C-HBCDs, the internal standards, were extracted using Soxhlet extraction, and further purified using acidic silica treatment and solid phase extraction. The separation of HBCDs was performed on Waters ACQUITY UPLCTM system with the column of BEH C18 and the gradient elution solvent of methanol-acetonitrile and water at a flow rate of 0.2 mL/min. The HBCDs were identified on the basis of the retention times and precursor ions, and quantitatively determined under the selected ion recording mode, m/z 640.7 for the [ M - H ]^ - ion. The limits of detection （LODs） of HBCDs ranged from 0. 1 to 0.4 ng/g; and the limits of quantification （LOQs） ranged from 0.4 to 1.2 ng/g. The average recoveries ranged from 92.9% to 99.3% for the spiked levels of 0.6, 2.0 and 6.0 ng/g, with the relative standard deviations （RSDs） between 3. 1% and 8.0%.

关 键 词：超高效液相色谱 电喷雾质谱 同位素稀释 六溴环十二烷异构体 食品 

分 类 号：O658[理学—分析化学]