GC-MS Determination of 8 Antibacterial Agents in Textiles with Single Drop Microextraction
摘 要
取剪成小片(5 mm×5 mm)的样品(1.00 g),于模拟汗液50 mL中,在50 ℃振荡浸泡2 h,冷却至室温,调节其酸度为pH 8.0。用微量进样器移取氯苯萃取剂2.0 μL,将进样器针尖置于浸泡液液面下方1 cm左右处并形成微液滴;在25 ℃和200 r·min-1的搅拌速率下萃取30 min。回收全部萃取液并用甲醇稀释至50 μL作为样品溶液。按所选仪器工作条件进行气相色谱-质谱分析。8种抗菌剂的质量浓度均在1.0~40 mg·L-1范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.08~0.24 mg·L-1之间。以空白样品为基体进行加标回收试验,所得回收率在83.6%~98.9%之间,测定值的相对标准偏差(n=6)在3.7%~9.1%之间。
Abstract
A portion of the sliced strip-sample (5 mm×5 mm, 1.00 g) was extracted by shaking with 50 mL of the simulated perspiration at 50 ℃ for 2 h. After cooling to room temperature, the acidity of the extract was adjusted to pH 8.0. 2.0 μL of the extractant-chlorobenzene were added into the perspiration extract using a microsampler with its syringe needle placed 1 cm below the solution surface level, and thence to form a microdroplet, and micro-extraction was performed by agitation at a rate of 200 r·min-1 for 30 min at 25 ℃. Whole of the chlorobenzene extract was recovered and diluted to 50 μL with methanol for use as sample solution in the following GC-MS analysis under prescribed conditions. Linear relationships between values of peak area and mass concentration of the 8 antibacterial agents were kept in the same range of 1.0-40 mg·L-1, with detection limits (3S/N) in the range of 0.08-0.24 mg·L-1. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 83.6%-98.9%, with RSDs (n=6) in the range of 3.7%-9.1%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201612003
所属栏目 试验与研究
基金项目 国家质量监督检验检疫总局科技计划项目(2014QK209)
收稿日期 2015/12/21
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备注陈兆波(1967-),男,浙江余姚人,高级工程师,主要从事产品检测和管理工作。
引用该论文: CHEN Zhao-bo,GU Hu,QIN Xin. GC-MS Determination of 8 Antibacterial Agents in Textiles with Single Drop Microextraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2016, 52(12): 1375~1379
陈兆波,顾虎,秦鑫. 单滴微萃取-气相色谱-质谱法测定纺织品中8种抗菌剂[J]. 理化检验-化学分册, 2016, 52(12): 1375~1379
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参考文献
【1】GONZALO L R, SANZ L J, CAMARA C. Analytical performance of two miniaturized extraction methods for triclosan and methyltriclosan,in fish roe and surimi samples[J]. Science of the Total Enviroment, 2014,472(2):235-238.
【2】储蕙,夏宝风.防霉剂α-溴代肉桂醛对皮肤刺激性和致敏性的探讨[J].中国工业医学杂志, 2000,13(3):149-150.
【3】王成云,谢堂堂,杨左军,等.超高效液相色谱法测定纺织品中三氯生的含量[J].分析测试学报, 2010,29(12):1231-1234.
【4】解娜,丁晓静,宋宝花,等.胶束电动毛细管色谱法同时测定复方化学消毒剂及日化产品中邻苯二甲醛、对氯间二甲基苯酚及三氯生[J].色谱, 2013,31(1):64-70.
【5】武婷,王超,王星,等.反相高效液相色谱法测定化妆品中的24种防腐剂[J].分析化学, 2007,35(10):1439-1443.
【6】芦春梅,牟峻,周博宇,等.基于液相色谱-串联质谱法纺织品中三氯生的普查分析[J].纺织学报, 2014,35(5):87-90.
【7】赵惠清,苏军,李伟,等.高效液相色谱法检测化妆品中的三氯生、三氯卡班[J].中国卫生检验杂志, 2014,24(20):2915-2917.
【8】潘建君,张晓婷,陆勋元,等.高效液相色谱法测定纺织品中三氯生的研究[J].印染助剂, 2014,31(10):50-52.
【9】冯伟,张代辉,张勋,等.QuEChERS法提取-气相色谱-串联质谱法测定生态纺织品中31种农药残留[J].理化检验-化学分册, 2015,51(10):1386-1392.
【10】王国庆,张东飞,王素方,等.气相色谱-质谱法测定水果中杀菌剂残留量[J].理化检验-化学分册, 2010,46(2):197-199.
【11】李志刚.基于固相萃取-高效液相色谱法的纺织品中三氯生的测定[J].纺织学报, 2014,35(3):98-102.
【12】王雨堃,李超,马晶军,等.单滴微萃取技术的研究及应用进展[J].化学通报, 2012,75(7):628-636.
【13】GB/T 3922-2013纺织品 色牢度试验 耐汗渍色牢度[S].
【14】ANDRE M, DAVID R L. Triclocarban, triclosan and its transformation product methyl triclosan in biosolids application[J]. Food Chemistry, 2014,146(3):141-148.
【2】储蕙,夏宝风.防霉剂α-溴代肉桂醛对皮肤刺激性和致敏性的探讨[J].中国工业医学杂志, 2000,13(3):149-150.
【3】王成云,谢堂堂,杨左军,等.超高效液相色谱法测定纺织品中三氯生的含量[J].分析测试学报, 2010,29(12):1231-1234.
【4】解娜,丁晓静,宋宝花,等.胶束电动毛细管色谱法同时测定复方化学消毒剂及日化产品中邻苯二甲醛、对氯间二甲基苯酚及三氯生[J].色谱, 2013,31(1):64-70.
【5】武婷,王超,王星,等.反相高效液相色谱法测定化妆品中的24种防腐剂[J].分析化学, 2007,35(10):1439-1443.
【6】芦春梅,牟峻,周博宇,等.基于液相色谱-串联质谱法纺织品中三氯生的普查分析[J].纺织学报, 2014,35(5):87-90.
【7】赵惠清,苏军,李伟,等.高效液相色谱法检测化妆品中的三氯生、三氯卡班[J].中国卫生检验杂志, 2014,24(20):2915-2917.
【8】潘建君,张晓婷,陆勋元,等.高效液相色谱法测定纺织品中三氯生的研究[J].印染助剂, 2014,31(10):50-52.
【9】冯伟,张代辉,张勋,等.QuEChERS法提取-气相色谱-串联质谱法测定生态纺织品中31种农药残留[J].理化检验-化学分册, 2015,51(10):1386-1392.
【10】王国庆,张东飞,王素方,等.气相色谱-质谱法测定水果中杀菌剂残留量[J].理化检验-化学分册, 2010,46(2):197-199.
【11】李志刚.基于固相萃取-高效液相色谱法的纺织品中三氯生的测定[J].纺织学报, 2014,35(3):98-102.
【12】王雨堃,李超,马晶军,等.单滴微萃取技术的研究及应用进展[J].化学通报, 2012,75(7):628-636.
【13】GB/T 3922-2013纺织品 色牢度试验 耐汗渍色牢度[S].
【14】ANDRE M, DAVID R L. Triclocarban, triclosan and its transformation product methyl triclosan in biosolids application[J]. Food Chemistry, 2014,146(3):141-148.
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