GC-MS Determination of 9 Organotins in Latex Products
摘 要
样品2.000 0 g经丙酮20 mL超声提取45 min,提取液用丙酮定容至25.0 mL。取上述溶液1.0 mL,加入乙酸盐缓冲溶液(pH 4.0)5 mL、20 g·L-1四乙基硼酸钠溶液2 mL,超声反应45 min后,再加入正己烷2 mL,涡旋混合30 s。取上层有机相经脱水、过滤后,以DB-35MS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0.8~50 mg·L-1内与其峰面积呈线性关系,检出限(3S/N)为0.18~0.87 mg·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%。
Abstract
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-35MS 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 (3S/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%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201804016
所属栏目 工作简报
基金项目 上海市质量技术监督局公益性科技项目(2016-22);全国橡胶与橡胶制品标准化技术委员会胶乳制品分技术委员会国家推荐性标准立项(20151878-T-606)
收稿日期 2017/4/1
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备注左莹,硕士,高级工程师,研究方向为轻工产品有害物质化学检测,zuoying@sqi.org.cn
引用该论文: ZUO Ying,SHI Jun,LIU Jun,YANG Jianping,LI Jiejun. GC-MS Determination of 9 Organotins in Latex Products[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(4): 455~461
左莹,施均,刘峻,杨建平,李洁君. 气相色谱-质谱法测定胶乳产品中9种有机锡的含量[J]. 理化检验-化学分册, 2018, 54(4): 455~461
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【4】胡贵祥,万益群,朱惠芳.SPME-GC/MS在线衍生测定尿液中多种有机锡化合物[J].南昌大学学报(理科版), 2015,39(5):463-466.
【5】李英,李彬,刘丽,等.气相色谱-质谱法同时测定聚氯乙烯塑料制品中的10种有机锡化合物[J].色谱, 2009,27(1):69-73.
【6】邓爱华,庞晋山,彭晓俊,等.气相色谱/双柱双检测器测定塑料制品中10种有机锡[J].分析测试学报, 2015,34(1):35-42.
【7】黄国兰,孙红文,戴树桂.巯基棉预富集、气相色谱-原子吸收联用技术测定水样中丁基锡化合物[J].中国环境科学, 1997,17(3):283-286.
【8】林鋆,朱峰,王明葵.加速溶剂萃取-高效液相色谱-电感耦合等离子体质谱法测定聚乳酸材料中4种有机锡化合物[J].质谱学报, 2014,35(5):454-460.
【9】王莉,王斌,罗海英,等.固相萃取结合气相色谱-质谱法测定皮革中的14种阻燃剂[J].分析测试学报, 2016,35(12):1548-1553.
【10】裘智钢,魏晓英,蒋付良,等.气相色谱-质谱法测定合成革原料聚氨酯中的有机锡[J].现代纺织技术, 2012,20(4):45-49.
【11】李艳明,胡勇杰,刘金华,等.气相色谱-质谱法测定纺织助剂中的有机锡[J].色谱, 2011,29(4):353-357.
【12】胡志国.气相色谱-质谱法测定纺织品中的有机锡[J].质谱学报, 2005,26(1):59-61.
【13】崔宗岩,葛娜,曹彦忠,等.乙基化衍生-顶空固相微萃取-气相色谱串联质谱法测定海水中的有机锡化合物[J].分析化学, 2013,41(12):1887-1892.
【14】ZACHARIADIS G A, ROSENBERG E. Determination of butyl-and phenyltin compounds in human urine by HS-SPME after derivatization with tetraethylborate and subsequent determination by capillary GC with microwave-induced plasma atomic emission and mass spectrometric detection[J]. Talanta, 2009,78(2):570-576.
【15】荆淼,于振花,王小如,等.高效液相色谱-电感耦合等离子体质谱技术测定海水中锡化学形态[J].分析化学, 2008,36(2):235-237.
【16】MORABITO R, MASSANISSO P, QUEVAUVILLER P. Derivatization methods for the determination of organotin compounds in environmental samples[J]. TrAC Trends in Analytical Chemistry, 2000,19(2/3):113-119.
【17】JONES-LEPP T L, K E VARNER, MARK M D, et al. Determination of organotins in water by micro liquid chromatography-electrospray/ion trap mass spectrometry[J]. Applied Organometallic Chemistry, 1999,13:881-889.
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