气相色谱-串联质谱法测定水产品中五氯苯酚及其钠盐的残留量
GC-MS/MS Determination of Residual Amounts of Pentachlorophenol and Its Sodium Salt in Aquatic Products
摘 要
样品中的五氯苯酚及其钠盐在硫酸（1+1）溶液中转化为五氯苯酚，经活化的HLB固相萃取小柱净化后，在碳酸钾溶液中经乙酸酐衍生生成五氯苯乙酸酯。提取液以TR-5MS毛细管色谱柱为固定相进行气相色谱分离，采用负化学电离源和选择反应监测模式进行质谱分析，内标法定量。五氯苯酚的质量浓度在0.20~20.0 μg·L-1范围内与其峰面积比呈线性，检出限（3S/N）为1.0 μg·kg-1。以空白河蟹、鳕鱼样品为基体，按标准加入法进行回收试验，回收率为78.0%~104%，测定值的相对标准偏差（n=6）为2.0%~12%。
固相萃取
五氯苯酚
水产品
GC-MS/MS
solid phase extraction
pentachlorophenol
aquatic product
Abstract
The target compound in the sample was converted into pentachlorophenol (PCP) in the presence of sulfuric acid (1+1) solution. The solution after extraction was purified on activated HLB solid phase extraction column, and then pentachlorphenylacetate (PCP-OAc) was derived from the reaction of PCP with acetic anhydride in the presence of potassium carbonate solution. The solution after extraction was separated by GC using TR-5MS capillary column as stationary phase. NCI and SRM were adopted in MS, and internal standard method was used for quantification. Linear relationship between values of peak area ratio and mass concentration of PCP was found in the range of 0.20-20.0 μg·L-1, with detection limit (3S/N) of 1.0 μg·kg-1. The blank samples of crab and codfish were used as matrix, and test for recovery was made by standard addition method, giving results in the range of 78.0%-104%, with RSDs (n=6) ranged from 2.0% to 12%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201707025
所属栏目 专题报道(质谱)
基金项目 江苏省自然科学基金项目（BK20141500）；江苏省农业科技自主创新资金[CX（15）1013；CX（15）1011]；江苏省属公益院所能力提升项目（BM2015018）
收稿日期 2016/7/8
修改稿日期
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备注朱晓华(1975-),女,江苏无锡人,高级工程师,研究方向为水产品质量安全检测与研究,xhz824@sina.com
引用该论文: ZHU Xiaohua,WANG Kai,XIA Liping,LIANG Qian,MENG Yong. GC-MS/MS Determination of Residual Amounts of Pentachlorophenol and Its Sodium Salt in Aquatic Products[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2017, 53(7): 860～864
朱晓华,王凯,夏丽萍,梁倩,孟勇. 气相色谱-串联质谱法测定水产品中五氯苯酚及其钠盐的残留量[J]. 理化检验－化学分册, 2017, 53(7): 860～864
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参考文献
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【2】Agency for Toxic Substances and Disease Registry (ATSDR). Toxicological profile for pentachlorophenol (update):report of Department of Health and Human Services[R]. Atlanta:DHHS, 2001:152-163.
【3】张彤晴,蒋丽娟,葛家春,等.五氯苯酚对渔业环境的危害与对策研究进展[J].江苏农业科技, 2007(4):256-259.
【4】史雅娟,吕永龙,任鸿昌,等.持久性有机污染物研究国际发展动态[J].世界科技研究与发展, 2003,25(2):73-78.
【5】余刚,黄俊,张彭义.持久性有机污染物:倍受关注的全球性环境问题[J].环境保护, 2001(4):37-39.
【6】张兵,郑明辉,刘芃岩,等.五氯酚在洞庭湖环境介质中的分布[J].中国环境科学, 2001,21(2):165-167.
【7】荣宝晶,崔杨卓.4-氨基安替比林法测定水样中的酚的探讨和改进[J].北方环境, 2005,30(2):72-74.
【8】TURNES M I, MEJUTO M C, CELA R. Determination of pentachlorophenol in water samples by capillary zone electrophoresis[J]. Journal of Chromatography A, 1996,733(1/2):395-404.
【9】NOGUERA P, MAQUIEIRA Á, PUCHADES R, et al. Development of an enzyme-linked immunosorbent assay for pentachlorophenol[J]. Analytica Chimica Acta, 2002,460(2):279-288.
【10】余宇燕,张叔玲,邹艳辉,等.五氯酚免疫层析检测试纸条的研究[J].分析测试学报, 2004,33(7):830-834.
【11】费志良,葛家春,吴军,等.气相色谱测定青虾、草鱼肌肉中五氯苯酚及其钠盐残留总量的方法[J].南京师大学报(自然科学版), 2004,27(3):70-73.
【12】薛辉利,张晓辉,杜建明,等.虾类中五氯苯酚残留的气相色谱分析[J].福建分析测试, 2009,18(3):64-65.
【13】池缔萍.固相微萃取气相色谱法测定水产品中五氯苯酚及其钠盐残留量[J].分析试验室, 2007,26(增1):321-323.
【14】梁倩,朱晓华,王凯,等.水产品中五氯苯酚及其钠盐含量的气相色谱内标测定法[J].水产学报, 2012,36(5):779-786.
【15】BECKER R, BUGE H G, WIN T. Determination of pentachlorophenol (PCP) in waste wood-method comparison by a collaborative trial[J]. Chemosphere, 2002,47(9):1001-1006.
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【17】曹锡忠,沈崇钰,蔡建和,等.气相色谱法测定纺织品中五氯苯酚残留量[J].理化检验-化学分册, 2003,39(3):144-146.
【18】陈骥,陈舜湖,张祖麟,等.毛细管气相色谱法测定鳌江表层沉积物中五氯酚和六氯酚[J].环境监测管理与技术, 2008,20(4):40-42.
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【20】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.
【21】RIBEIRO A, NEVES M H, ALMEIDA M F, et al. Direct determination of chlorophenols in landfill leachates by solid-phase micro-extraction-gas chromatography-mass spectrometry[J]. Journal of Chromatography A, 2002,975(2):267-274.
【22】刘娅琳,吴笛,吴慧.在线衍生化吹扫捕集-气相色谱/质谱分析水中的五氯酚[J].中国环境管理干部学院学报, 2007,17(4):80-82.
【23】LACORTE S, GUILLAMON M. Validation of a pressurized solvent extraction and GC-NCI-MS method for the low level determination of 40 polybrominated diphenyl ethers in mothers' milk[J]. Chemosphere, 2008,73(1):70-75.
【24】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.
【25】沈登辉,章清荷,王冰霜,等.饮用水中五氯酚的固相萃取-气相色谱串联质谱测定法[J].环境与健康杂志, 2014,31(1):51-53.
【26】廖林川,颜有仪,林岚,等.高效液相色谱法检测生物样品中五氯酚[J].四川大学学报(医学版), 2004,35(3):427-428.
【27】JIN M C, ZHU Y. Ion chromatography-atmospheric pressure chemical ionization mass spectrometry for the determination of trace chlorophenols in clam tissues[J]. Journal of Chromatography A, 2006,1118(1):111-117.
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