顶空固相微萃取-气相色谱-质谱法测定二苯甲酮类防晒剂中残留溶剂
GC-MS Determination of Residual Solvent in Benzophenones Used as Tanning Preventives with Head-space SPME
摘 要
利用顶空固相微萃取-气相色谱-质谱联用技术,采用选择离子储存模式对2-羟基-4-甲氧基二苯甲酮-5-磺酸防晒剂中1,2-二氯乙烷残留溶剂进行测定,考虑基体效应的影响,采用乙烯二醇-二乙烯基苯共聚物(CW/DVB)固相微萃取纤维,通过标准加入法得到2-羟基-4-甲氧基二苯甲酮-5-磺酸中1,2-二氯乙烷残留量.方法的检出限(3S/N)为0.06 μg·g-1,回收率在99.0%~107.7%,相对标准偏差(n=5)为7.84%,线性范围为2.5~250 μg·g-1,该方法可用于药物中微量溶剂残留的测定.
顶空固相微萃取
残留溶剂
1,2-二氯乙烷
2-羟基-4-甲氧基二苯甲酮-5-磺酸
Hyphenation of GC and MS
Head-space-solid phase microextraction
Residual solvent
1,2-Dichloroethane
2-Hydroxy-4-methoxy-benzophenone-5-sulfonic acid
Abstract
The residual solvent,1,2-dichloroethane in a tanning preventive,2-hydroxy-4-methoxy-benzophenone-5-sulfonic acid (also known as benzophenone-4) was determined by GC-MS,with head-space solid phase micro-extraction (HS-SPME) and SIS mode. Copolymer of ethylene glycol and divinylbenzene (CW/DVB) was used as extracting fiber in SPME and method of standard addition as well as calculation by extrapolation were applied to eliminate the matrix effect. Linear relationship between values of peak area and mass fraction (w) of 1,2-dichloroethane was obtained in the range of 2.5 to 250 μg·g-1,and detection limit (3S/N) found for the method was 0.06 μg·g-1. Test for recovery was performed by analyzing a known sample for 5 determinations by the proposed method,values of recovery found were range from 99.0%-107.7%. Precision of the method was also tested,and the value of RSD (n=5) obtained was 7.84%.
中图分类号 O652.6
所属栏目 工作简报
基金项目 国家自然科学基金资助项目(30500339);浙江省自然科学基金资助项目(Y407308)
收稿日期 2008/11/16
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备注李祖光(1971-),男,江西上饶人,博士,教授,主要从事分析化学等的教学和科研工作.
引用该论文: LI Zu-guang,ZHU Guo-hua,CAO Hui,MO Wei-min. GC-MS Determination of Residual Solvent in Benzophenones Used as Tanning Preventives with Head-space SPME[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2009, 45(12): 1422～1423
李祖光,朱国华,曹慧,莫卫民. 顶空固相微萃取-气相色谱-质谱法测定二苯甲酮类防晒剂中残留溶剂[J]. 理化检验－化学分册, 2009, 45(12): 1422～1423
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【5】钱君律,林宁,邓志华.紫外线吸收剂UV-9生产新工艺[J].上海化工,2000,7:15-16．
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【11】LI Zu-guang,LEE Maw-rong,SHEN De-long. Analysis of volatile compounds emitted from fresh Syringa oblata flowers in different florescence by headspace solid-phase microextraction-gas chromatography-mass spectrometry[J]. Anal Chim Acta,2006,576(1):43-49．
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