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

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0.06μg·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2.5～250μg·g^(-1),该方法可用于药物中微量溶剂残留的测定。

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. 06μg · 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%.