气相色谱-质谱法测定涂料中的六溴环十二烷
GC-MS Determination of Hexabromocyclododecane in Coatings
摘 要
提出了用气相色谱-质谱法测定涂料中六溴环十二烷含量的方法。样品用二氯甲烷-丙酮(1+1)混合溶剂超声提取,提取液经硅胶固相萃取小柱净化、平行蒸发定量浓缩后,用DB-5MS毛细管柱进行分离,全扫描模式和选择离子监测模式测定。六溴环十二烷的质量浓度在1~50 mg·L-1范围内与其峰面积呈线性关系,测定下限(10S/N)为10 mg·kg-1。添加5,20,50 mg·L-1 3个浓度水平进行加标回收试验,回收率在82.0%~106%之间,测定值的相对标准偏差(n=8)在2.8%~5.3%之间。
六溴环十二烷
涂料
GC-MS
Hexabromocyclododecane
Coating
Abstract
A method for the determination of hexabromocyclododecane (HBCD) in coatings by GC-MS was proposed. Sample was ultrasonically extracted with dichloromethane-acetone (1+1) mixed solvent, purified by passing through silica gel solid phase extraction column, and quantitatively concentrated with parallel evaporation instrument. DB-5MS capillary column was used for separation, and full-scanning mode and selected ion monitoring mode were adopted in MS determination. Linear relationship between values of peak area and mass concentration of HBCD was kept in the range of 1-50 mg·L-1, with lower limit of determination (10S/N) of 10 mg·kg-1. Tests for recovery were made at the concentration levels of 5, 20, 50 mg·L-1 of HBCD standard, giving values of recovery and RSD′s (n=8) in the ranges of 82.0%-106% and 2.8%-5.3% respectively.
中图分类号 O657.63
所属栏目 工作简报
基金项目 “十二五”国家科技支撑计划项目(2012BAK26B04);质检公益性行业科研专项(201010073-03);国家质检总局科研项目(2010IK039)
收稿日期 2011/5/9
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备注唐志锟(1983-),男,广东佛山人,工程师,从事进出口商品检验工作。
引用该论文: TANG Zhi-kun,CHEN Qiang,LI Dan,ZHOU Ming-hui,LIU Ying-feng,ZHAI Cui-ping,ZHENG Jian-guo,ZHONG Zhi-guang. GC-MS Determination of Hexabromocyclododecane in Coatings[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2012, 48(7): 807～809
唐志锟,陈强,李丹,周明辉,刘莹峰,翟翠萍,郑建国,钟志光. 气相色谱-质谱法测定涂料中的六溴环十二烷[J]. 理化检验－化学分册, 2012, 48(7): 807～809
被引情况:
【1】阮毅,叶典贤,方正, "碳骨架-气相色谱法测定电子电气材料中六溴环十二烷",理化检验－化学分册 51, 1093-1095(2015)
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【13】杜伟.高效液相色谱-串联质谱法分析六溴环十二烷对映异构体［J］.环境化学, 2011,30(10):1833-1834.
【14】岳强.环境中六溴环十二烷的研究现状与展望［J］.广东农业科学, 2010(6):217-220.
【2】European Chemicals Agency. Proposals to identify substances of very high concern: annex XV reports previously commented by interested parties. http://echa.europa.eu/consultations/authorisation/svhc/svhc_prev_cons_en.asp.
【3】梁元媛.解读挪威PoHS禁令［J］.电子质量, 2008(4):78-80.
【4】HAUG L S, THOMSEN C, LIANE V H, et al. Comparison of GC and LC determinations of hexabromocyclododecane in biological samples-results from two interlaboratory comparison studies［J］. Chemosphere, 2008,71(6):1087-1092.
【5】HIEBI J, VETTER W. Detection of hexabromocyclododecane and its metabolite pentabromocyclododecene in chicken egg and fish from the official food control［J］. J Agric Food Chem, 2007,55(9):3319-3324.
【6】潘荷芳,惠阳,王静,等.土壤中痕量六溴环十二烷的超高效液相色谱-质谱联用分析［J］.分析科学学报, 2008,24(4):414-416.
【7】YU Zhi-qiang, PENG Ping-an, SHENG Guo-ying, et al. Determination of hexabromocyclododecane diastereoisomers in air and soil by liquid chromatography-electrospray tandem mass spectrometry［J］. J Chromatogr A, 2008,1190(1):74-79.
【8】GUERRA P, ELJARRAT E, BARCEL D. Enantiomeric specific determination of hexabromocyclododecane by liquid chromatography-quadrupole linear ion trap mass spectrometry in sediment samples［J］. J Chromatogr A, 2008,1203(1):81-87.
【9】施致雄,封锦芳,李敬光,等.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［J］.色谱, 2008,26(1):1-5.
【10】金军,杨从巧,王英,等.超高效液相色谱-电喷雾离子源-串联三重四极质谱分析土壤中六溴环十二烷［J］.分析化学, 2009,37(4):585-588.
【11】马强,白桦,王超,等.同位素稀释-超高效液相色谱-串联质谱法测定纺织品中的六溴环十二烷［J］.高等学校化学学报, 2010,31(3):473-478.
【12】韩超,贾婉娉,朱振瓯,等.加速溶剂萃取-固相萃取-液相色谱-电喷雾串联质谱法同时测定羊栖菜中六溴环十二烷异构体［J］.分析试验室, 2011,30(1):59-62.
【13】杜伟.高效液相色谱-串联质谱法分析六溴环十二烷对映异构体［J］.环境化学, 2011,30(10):1833-1834.
【14】岳强.环境中六溴环十二烷的研究现状与展望［J］.广东农业科学, 2010(6):217-220.
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