气相色谱-质谱法测定胶乳产品中9种有机锡的含量

GC-MS Determination of 9 Organotins in Latex Products

样品2.000 0g经丙酮20mL超声提取45min,提取液用丙酮定容至25.0mL。取上述溶液1.0mL,加入乙酸盐缓冲溶液(pH 4.0)5mL、20g·L^(-1)四乙基硼酸钠溶液2mL,超声反应45min后,再加入正己烷2mL,涡旋混合30s。取上层有机相经脱水、过滤后,以DB^(-3)5MS色谱柱为固定相,采用气相色谱分离9种有机锡。质谱分析中采用电子轰击离子源(EI)和选择离子监测模式(SIM)。9种有机锡的质量浓度在0.8~50mg·L^(-1)内与其峰面积呈线性关系,检出限(3S/N)为0.18~0.87mg·kg^(-1)。按标准加入法进行回收试验,回收率为82.0%~105%,相对标准偏差(n=6)均小于7.0%。

The sample（2.000 0 g）was extracted ultrasonically with acetone of 20 mL for 45 min,and the extract was made its volume up to 25.0 mL with acetone.The above solution of 1.0 mL was taken,and acetic acid buffer solution（pH 4.0）of 5 mL and 20 g·L^-1 sodium tetraethylborate solution of 2 mL were added.After ultrasonic reaction for 45 min,hexane of 2 mL was added and then the mixture was mixed whirly for 30 s.After dehydration and filtration of the upper layer organic phase,9 organotins were separated by gas chromatography（GC）with DB^-35 MS column as the stationary phase.EI and SIM were adopted in MS analysis.Linear relationships between peak area and mass concentration of 9 organotins were found in the range of 0.8-50 mg·L^-1,with detection limits（3 S/N）in the range of 0.18-0.87 mg·kg^-1.Tests for recovery were made by standard addition method,giving results in the range of 82.0%^-105%,with RSDs（n=6）all less than 7.0%.