旋涡辅助-柱前衍生-气相色谱-串联质谱法测定木砧板及木筷子中的五氯酚
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摘要
目的建立旋涡辅助-柱前衍生-气相色谱-串联质谱(GC-MS/MS)法测定木砧板及木筷子中五氯酚的方法。方法加入硫酸溶液,使五氯酚钠转化为分子态的五氯酚,以乙酸乙酯-正己烷混合溶剂(2∶8,V/V)萃取,浓硫酸净化,加入乙酸酐吡啶溶液衍生。采用HP-5MS色谱柱(30 m×0.25 mm,0.25μm)进行分离,GC-MS-MS多反应监测(MRM)测定。结果在0～200μg/L范围内,五氯酚具有良好的线性关系(r=0.999 8),检出限为0.2μg/kg,定量限为0.7μg/kg。在高、中、低3个浓度水平下,平均加标回收率为90.0%～103.6%,相对标准偏差(RSD)为1.5%～3.6%(n=6)。结论本方法具有准确性高、灵敏度高、快速等特点,适用于木砧板及木筷子中五氯酚的准确检测。
Objective To establish a method for the determination of pentachlorophenol in wooden chopping boards and wooden chopsticks by vortex-assisted pre-column derivatization gas chromatography-tandem mass spectrometry(GC-MS/MS). Methods The sulfuric acid solution was added to convert sodium salt into molecular pentachlorophenol, which was extracted with a mixed solvent of ethyl acetate and n-hexane(2∶8,V/V), purified by concentrated sulfuric acid, and derivatized with acetic acid pyridine solution. HP-5 MS column(30 m×0.25 mm,0.25 μm) was used for separation and GC-MS/MS multiple reaction monitoring(MRM) was used for determination. Results In the range of 0-200 μg/L, pentachlorophenol had a good linear relationship(r=0.999 8), the detection limit was 0.2 μg/kg, and the limit of quantification was 0.7 μg/kg. The recoveries and precisions of the three concentrations(n=6) showed an average spike recovery ranged from 90.0% to 103.6% with the relative standard deviation(RSD) of 1.5%-3.6%. Conclusion This method was accurate, highly sensitive and rapid. It is suitable for the accurate detection of pentachlorophenol in wooden chopping boards and wooden chopsticks.
Objective To establish a method for the determination of pentachlorophenol in wooden chopping boards and wooden chopsticks by vortex-assisted pre-column derivatization gas chromatography-tandem mass spectrometry(GC-MS/MS). Methods The sulfuric acid solution was added to convert sodium salt into molecular pentachlorophenol, which was extracted with a mixed solvent of ethyl acetate and n-hexane(2∶8,V/V), purified by concentrated sulfuric acid, and derivatized with acetic acid pyridine solution. HP-5 MS column(30 m×0.25 mm,0.25 μm) was used for separation and GC-MS/MS multiple reaction monitoring(MRM) was used for determination. Results In the range of 0-200 μg/L, pentachlorophenol had a good linear relationship(r=0.999 8), the detection limit was 0.2 μg/kg, and the limit of quantification was 0.7 μg/kg. The recoveries and precisions of the three concentrations(n=6) showed an average spike recovery ranged from 90.0% to 103.6% with the relative standard deviation(RSD) of 1.5%-3.6%. Conclusion This method was accurate, highly sensitive and rapid. It is suitable for the accurate detection of pentachlorophenol in wooden chopping boards and wooden chopsticks.
引文
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[15] 唐晓琴,胡黎黎,顾万江.超高效液相色谱-四极杆-静电场轨道阱高分辨质谱法测定猪肉中的五氯酚[J].中国卫生检验杂志,2018,28(2):139-141,154.
[16] AMENDOLA L,CORTESEA M,VINATORU D,et al.Innov-ative analytical method for the determination of underivatized trib-utyltin and pentachlorophenol in seawater by gas chromatography-triple quadrupole mass spectrometry[J].Anal Chim Acta,2017,975(4):70-77.
[17] 赵舰,程莉,唐晓琴,等.气相色谱-离子阱质谱(MS～n)同位素内标衍生法测定鸡肉和猪肉中的五氯酚[J].中国卫生检验杂志,2016,26(19):2773-2775.
[18] 何雄,周静峰,汤海青.固相萃取-气相色谱-串联质谱法测定淡水鱼鱼肉中的五氯酚[J].食品安全质量检测学报,2018,9(9):2096-2100.
[19] 王虹,李跃红.HPLC法测定柞木中的五氯酚钠[J].中国食品卫生杂志,1997,9(2):14-15.
[20] 黄惠玲,何志贵,李渺,等.木材及木制品中残留五氯酚的气相色谱测定法[J].分析化学,2007,35(9):1369-1372.
[21] 黄姣,马明,肖玲艳,等.加速溶剂萃取-气相色谱法测定木材中五氯酚残留量[J].理化检验-化学分册,2013,49(2):174-176.
[22] 王连珠,方恩华,王彩娟,等.QuEChERS-超高效液相色谱-串联质谱法测定动物源食品中痕量五氯酚及其钠盐[J].色谱,2018,36(6):518-522.
[2] 胡林林,李鱼,耿辉,等.紫外分光光度法测定水样中五氯酚[J].吉林大学学报(理学版),2007,45(2):320-323.
[3] 吕月宾,方燕.固相萃取-高效液相色谱法测定饮用水中2,4-二氯酚、2,4,6-三氯酚、五氯酚[J].科技与企业,2012(15):355.
[4] 李小敏,何佶.固相萃取-高效液相色谱法测定水中酚同系物[J].理化检验-化学分册,2008,44(11):1105-1107.
[5] 端礼钦,王静,刘孝德,等.气相色谱内标法测定水产品中五氯酚[J].理化检验-化学分册,2011,47(11):1307-1309.
[6] DOMENO C,MUNIZZA G,NERIN C.Development of a solid-phase microextraction method for direct determination of pentachlorophenol in paper and board samples:comparison with conventional extraction method[J].J Chromatogr A,2005,1095(1/2):8-15.
[7] YU X S,LIU Y,LOU J,et al.Determination of water-and methanol-extractable pentachlorophenol in soils using vortex-assisted liquid-liquid extraction and gas chromatography[J].Chinese Journal of Analytical Chemistry,2015,43(9):1389-1394.
[8] 蒋红进,周美玲,王丽君.气相色谱法测定鱼体中残留五氯酚及其盐类[J].中国卫生检验杂志,2010,20(10):2432-2433,2436.
[9] 张渊,谢萍娟,刘芬,等.气相色谱法测定沉积物中三氯酚和五氯酚[J].山西农业科学,2016,44(6):805-807,847.
[10] MORALES R,CRUZ O M,SARABIA L A.Optimization of headspace experimental factors to determine chlorophenols in water by means of headspace solid-phase microextraction and gas chromatography coupled with mass spectrometry and parallel factor analysis[J].Anal Chim Acta,2012,754(10):20-30.
[11] 史玉坤,杨梅桂,杨清华,等.气相色谱-质谱法快速检测水产品中五氯酚[J].中国食品卫生杂志,2015,27(1):19-21.
[12] ZHOU Y,JIANG Q W,PENG Q,et al.Development of a solid phase microextraction-gas chromatography-mass spectrometry method for the determination of pentachlorophenol in human plasma using experimental design[J].Chemosphere,2007,70(2):256-262.
[13] KADMI Y,FAVIER L,WOLBERT D,et al.A new strategy for pentachlorophenol monitoring in water samples using ultra-high performance liquid chromatography-tandem mass spectrometry[J].Environ Eng Manage J,2015,14(3):567-574.
[14] 陈晓红,潘胜东,金米聪.固相萃取-超快速液相色谱串联质谱测定食品中五氯酚[J].卫生研究,2018,47(3):440-445,458.
[15] 唐晓琴,胡黎黎,顾万江.超高效液相色谱-四极杆-静电场轨道阱高分辨质谱法测定猪肉中的五氯酚[J].中国卫生检验杂志,2018,28(2):139-141,154.
[16] AMENDOLA L,CORTESEA M,VINATORU D,et al.Innov-ative analytical method for the determination of underivatized trib-utyltin and pentachlorophenol in seawater by gas chromatography-triple quadrupole mass spectrometry[J].Anal Chim Acta,2017,975(4):70-77.
[17] 赵舰,程莉,唐晓琴,等.气相色谱-离子阱质谱(MS～n)同位素内标衍生法测定鸡肉和猪肉中的五氯酚[J].中国卫生检验杂志,2016,26(19):2773-2775.
[18] 何雄,周静峰,汤海青.固相萃取-气相色谱-串联质谱法测定淡水鱼鱼肉中的五氯酚[J].食品安全质量检测学报,2018,9(9):2096-2100.
[19] 王虹,李跃红.HPLC法测定柞木中的五氯酚钠[J].中国食品卫生杂志,1997,9(2):14-15.
[20] 黄惠玲,何志贵,李渺,等.木材及木制品中残留五氯酚的气相色谱测定法[J].分析化学,2007,35(9):1369-1372.
[21] 黄姣,马明,肖玲艳,等.加速溶剂萃取-气相色谱法测定木材中五氯酚残留量[J].理化检验-化学分册,2013,49(2):174-176.
[22] 王连珠,方恩华,王彩娟,等.QuEChERS-超高效液相色谱-串联质谱法测定动物源食品中痕量五氯酚及其钠盐[J].色谱,2018,36(6):518-522.