Li Yanming, Hu Yongjie, Liu Jinhua, Guo Yuliang, Wang Guiqin
Dymatic Chemicals, Inc., Shunde 528305, China.
Se Pu. 2011 Apr;29(4):353-7. doi: 10.3724/sp.j.1123.2011.00353.
A gas chromatography-mass spectrometry (GC-MS) method has been developed for the determination of dibutyltin (DBT), tributyltin (TBT) and triphenyltin (TPhT) in textile auxiliaries. The sample was first extracted with n-hexane in acetate buffer solution (pH 4.0) under ultrasonication (for hydrophobic sample) or oscillation extraction (for hydrophilic sample) and then derivatized with sodium tetraethylborate in tetrahydrofuran. The derivative was determined by GC-MS in selected ion monitoring (SIM) mode. The separation and quantification were achieved using a Rxi-5 ms silica capillary column (30 m x 0.25 mm x 0.25 microm). The linear ranges were 0.1-8.0 mg/L for both DBT and TBT, and 0.1-4.0 mg/L for TPhT. There were good linear relationships between the peak area and concentration in the linear ranges and the correlation coefficients (r2) were 0.9994-0.9998. The detection limits (LOD) were from 0.003 mg/L to 0.005 mg/L. The average recoveries of these organotin compounds at the three spiked levels of 4.0, 10.0 and 40.0 mg/kg were 92.6%-108.0% with the relative standard deviations (RSDs) of 2.5%-10.2%. The method is simple and accurate for simultaneous analysis of the DBT, TBT and TPhT in textile auxiliaries.
已开发出一种气相色谱 - 质谱联用(GC-MS)方法,用于测定纺织助剂中的二丁基锡(DBT)、三丁基锡(TBT)和三苯基锡(TPhT)。首先,将样品在乙酸盐缓冲溶液(pH 4.0)中用正己烷超声提取(用于疏水性样品)或振荡萃取(用于亲水性样品),然后在四氢呋喃中用四乙基硼酸钠进行衍生化。衍生物通过GC-MS在选择离子监测(SIM)模式下进行测定。使用Rxi-5 ms硅胶毛细管柱(30 m×0.25 mm×0.25 µm)实现分离和定量。DBT和TBT的线性范围均为0.1 - 8.0 mg/L,TPhT的线性范围为0.1 - 4.0 mg/L。在这些线性范围内,峰面积与浓度之间具有良好的线性关系,相关系数(r2)为0.9994 - 0.9998。检测限(LOD)为0.003 mg/L至0.005 mg/L。在4.0、10.0和40.0 mg/kg三个加标水平下,这些有机锡化合物的平均回收率为92.6% - 108.0%,相对标准偏差(RSD)为2.5% - 10.2%。该方法简单准确,可同时分析纺织助剂中的DBT、TBT和TPhT。