Determination of Pentachlorophenol on the Surface of Wooden Chopping Board by Gas Chromatography-Tandem Mass Spectrometry
摘 要
建立了气相色谱-串联质谱法测定竹木砧板中五氯酚含量的方法。通过表层取样法与九点式布点法联合制备样品后,在2.00 g样品中加入10.0 mg·L-1的2,4,6-三溴酚内标溶液50 μL,以体积比1∶9的乙酸乙酯-正己烷混合液10 mL为提取剂,经SLC固相萃取柱净化后,洗脱液氮吹至1.0 mL,用体积比1∶1的乙酸酐-吡啶混合液进行衍生。样品衍生后,在Agilent J&W DB-5MS石英毛细管色谱柱上采用柱升温程序进行分离。质谱分析中采用多反应监测模式检测,内标法定量。结果表明:五氯酚的质量浓度在25~800 μg·L-1内与五氯酚衍生物和2,4,6-三溴酚衍生物的峰面积比值呈线性关系,检出限(3S/N)为0.003 mg·kg-1。按标准加入法进行回收试验,测得回收率为86.0%~96.0%,测定值的相对标准偏差(n=5)均小于5.0%。按此方法对80份竹木砧板样品开展食品安全风险专项监测,发现非定型包装竹木砧板中五氯酚高残留量(高达384.350 mg·kg-1)的风险隐患,为相关部门提供了风险预警。
Abstract
A method was established for the determination of pentachlorophenol in wooden chopping board by gas chromatography-tandem mass spectrometry (GC-MS/MS). The samples were prepared by the surface sampling method and the nine-point layout method. 2,4,6-tribromophenol internal standard solution of 10.0 mg·L-1 (50 μL) was added into the sample of 2.00 g, and a mixture of ethyl acetate and n-hexane at volume ratio of 1∶9 (10 mL) was used as the extractant. After purification by SLC solid phase extraction column, the eluent was blown to 1.0 mL with nitrogen, and a mixture of acetic anhydride and pyridine at volume ratio of 1∶1 was used for derivatization. After derivatization, the sample was separated on Agilent J&W DB-5MS quartz capillary column by column temperature program. The mode of multireaction monitoring (MRM) was adopted in MS/MS, and internal standard method was used for quantitative analysis. The results showed that linear relationship between peak area ratio of pentachlorophenol derivative and 2,4,6-tribromophenol derivative and mass concentration of pentachlorophenol was found in the range of 25-800 μg·L-1, with detection limit (3S/N) of 0.003 mg·kg-1. Test for recovery was made by standard addition method, giving results in the range of 86.0%-96.0%, and RSDs (n=5) of the determined values less than 5.0%. This method was used to carry out special food safety risk monitoring on 80 samples of wooden chopping board, and the hidden risk of high residues of pentachlorophenol (up to 384.350 mg·kg-1) in non-shaped packaging wooden chopping boards was discovered, which provided risk early warning for relevant departments.
中图分类号 O657.63 R115 DOI 10.11973/lhjy-hx202110003
所属栏目 工作简报
基金项目 贵州省疾病预防控制中心青年基金(2019-E2-8青);国家重点研发计划,食品安全预警监测及风险管控大数据应用服务平台构建与应用示范(2017YFC1601806);贵州省科技基础条件平台专项计划(黔科合平台人才[2016]5705);贵州省科技支撑计划(黔科合支撑[2017]2972)
收稿日期 2020/5/10
修改稿日期
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联系人作者陈庆园(jkzxcqy@126.com)
备注张权,技师,硕士,主要从事色谱与质谱分析研究工作
引用该论文: ZHANG Quan,LIU Liya,WU Yutian,LI Lei,LIU Wenzheng,GUO Hua,CHEN Qingyuan. Determination of Pentachlorophenol on the Surface of Wooden Chopping Board by Gas Chromatography-Tandem Mass Spectrometry[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2021, 57(10): 879~884
张权,刘利亚,吴玉田,李磊,刘文政,郭华,陈庆园. 气相色谱-串联质谱法测定竹木砧板表层中五氯酚的含量[J]. 理化检验-化学分册, 2021, 57(10): 879~884
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参考文献
【1】BRODEUR J C, GEORGE D D, SCOTT M R. Inhibition of oxygen consumption by pentachlorophenol and tetrachloroguaiacol in rainbow trout (Oncorhynchus mykiss)[J]. Aquatic Toxicology, 2001, 54(1/2):143-148.
【2】BOURDAT-DESCHAMPS M, LEANG S, BERNET N, et al. Multi-residue analysis of pharmaceuticals in aqueous environmental samples by online solid-phase extraction-ultra-high-performance liquid chromatography-tandem mass spectrometry:Optimisation and matrix effects reduction by quick, easy, cheap, effective, rugged and safe extraction[J]. Journal of Chromatography A, 2014, 1349:11-23.
【3】周敏, 朱萌萌, 周婷婷, 等.液液萃取-磺化净化-LC/MS/MS测定黄喉中的五氯酚酸钠[J].食品工业, 2019, 40(3):280-284.
【4】郑晓峰, 李鹏鹏, 张晓霞, 等.液液萃取-液相色谱法测定饮用水中的2, 4, 6-三氯酚和五氯酚[J].城镇供水, 2019(2):27-29.
【5】FENG Q Z, ZHAO L X, YAN W, et al. Molecularly imprinted solid-phase extraction combined with high performance liquid chromatography for analysis of phenolic compounds from environmental water samples[J]. Journal of Hazardous Materials, 2009, 167(1/2/3):282-288.
【6】DOMEÑO C, MUNIZZA G, NERÍN C. Development of a solid-phase microextraction method for direct determination of pentachlorophenol in paper and board samples:Comparison with conventional extraction method[J]. Journal of Chromatography 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】AMENDOLA L, CORTESE M, VINATORU D, et al. Innovative analytical method for the determination of underivatized tributyltin and pentachlorophenol in seawater by gas chromatography-triple quadrupole mass spectrometry[J]. Analytica Chimica Acta, 2017, 975:70-77.
【9】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]. Analytica Chimica Acta, 2012, 754:20-30.
【10】李启, 徐峻卿, 纪律.液液萃取-超高效液相色谱-串联质谱法测定砧板中五氯酚钠[J].中国食品卫生杂志, 2019, 31(3):236-239.
【11】田春霞, 金绍强, 朱炳祺, 等.超高效液相色谱-电喷雾串联质谱测定动物源食品中五氯酚的残留量[J].分析试验室, 2019, 38(4):438-441.
【12】FAVIER L, KADMI Y, HARJA M, et al. A new strategy for pentachlorophenol monitoring in water samples using ultra-high performance liquid chromatography-mass spectrometry tandem[J]. Environmental Engineering and Management Journal, 2015, 14(3):567-574.
【13】杨平华, 陈小艳, 张新华, 等.气相色谱法测定鄱阳湖湿地多种环境介质中五氯酚钠[J].理化检验-化学分册, 2018, 54(11):1246-1249.
【14】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.
【15】张志荣, 张来颖, 王玉江, 等.高效液相色谱-串联质谱法测定食品用纸制品中氯酚类化合物残留量[J].中国食品卫生杂志, 2019, 31(3):226-230.
【16】兰红军, 吴雪梅, 冯耀基, 等.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[J].中国食品卫生杂志, 2019, 31(3):231-236.
【17】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】BOURDAT-DESCHAMPS M, LEANG S, BERNET N, et al. Multi-residue analysis of pharmaceuticals in aqueous environmental samples by online solid-phase extraction-ultra-high-performance liquid chromatography-tandem mass spectrometry:Optimisation and matrix effects reduction by quick, easy, cheap, effective, rugged and safe extraction[J]. Journal of Chromatography A, 2014, 1349:11-23.
【3】周敏, 朱萌萌, 周婷婷, 等.液液萃取-磺化净化-LC/MS/MS测定黄喉中的五氯酚酸钠[J].食品工业, 2019, 40(3):280-284.
【4】郑晓峰, 李鹏鹏, 张晓霞, 等.液液萃取-液相色谱法测定饮用水中的2, 4, 6-三氯酚和五氯酚[J].城镇供水, 2019(2):27-29.
【5】FENG Q Z, ZHAO L X, YAN W, et al. Molecularly imprinted solid-phase extraction combined with high performance liquid chromatography for analysis of phenolic compounds from environmental water samples[J]. Journal of Hazardous Materials, 2009, 167(1/2/3):282-288.
【6】DOMEÑO C, MUNIZZA G, NERÍN C. Development of a solid-phase microextraction method for direct determination of pentachlorophenol in paper and board samples:Comparison with conventional extraction method[J]. Journal of Chromatography 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】AMENDOLA L, CORTESE M, VINATORU D, et al. Innovative analytical method for the determination of underivatized tributyltin and pentachlorophenol in seawater by gas chromatography-triple quadrupole mass spectrometry[J]. Analytica Chimica Acta, 2017, 975:70-77.
【9】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]. Analytica Chimica Acta, 2012, 754:20-30.
【10】李启, 徐峻卿, 纪律.液液萃取-超高效液相色谱-串联质谱法测定砧板中五氯酚钠[J].中国食品卫生杂志, 2019, 31(3):236-239.
【11】田春霞, 金绍强, 朱炳祺, 等.超高效液相色谱-电喷雾串联质谱测定动物源食品中五氯酚的残留量[J].分析试验室, 2019, 38(4):438-441.
【12】FAVIER L, KADMI Y, HARJA M, et al. A new strategy for pentachlorophenol monitoring in water samples using ultra-high performance liquid chromatography-mass spectrometry tandem[J]. Environmental Engineering and Management Journal, 2015, 14(3):567-574.
【13】杨平华, 陈小艳, 张新华, 等.气相色谱法测定鄱阳湖湿地多种环境介质中五氯酚钠[J].理化检验-化学分册, 2018, 54(11):1246-1249.
【14】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.
【15】张志荣, 张来颖, 王玉江, 等.高效液相色谱-串联质谱法测定食品用纸制品中氯酚类化合物残留量[J].中国食品卫生杂志, 2019, 31(3):226-230.
【16】兰红军, 吴雪梅, 冯耀基, 等.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[J].中国食品卫生杂志, 2019, 31(3):231-236.
【17】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.
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