Abstract
In order to develop a method for the determination of trace pentachlorophenol and its sodium salt in animal-origin foods by automated solid phase extraction-coupled with ultra performance liquid chromatography-tandem mass spectrometry, the effects of extractive solvents, solid phase extraction columns, eluents, mass spectrum and chromatographic separation conditions, internal standards were studied and compared. Finally, the sample was extracted by 5% ammonia acetonitrile, purified by MAX solid phase extraction column and eluted by 10% formic acid methanol. The extract was dried-up with nitrogen and re-dissolved with acetonitrile water solution (50∶50).The solution was separated on a Kinetex C18 column (100 mm×2.1 mm, 2.6 μm) with gradient elution program of acetonitrile and 5mmol/L ammonium acetate (0.1% formic acid) as the mobile phase. The detection was performed by UPLC-MS/MS using the negative electrospray ionization interface under the multiple reaction monitoring mode (MRM), and quantified with internal standard method. The developed method showed a good linearity in the range of 0.2~10.0 μg/L, with correlation coefficients (r) above 0.999. The mean recoveries spiked at levels of 1.0, 5.0, 10.0 μg/kg were within 86.0%~106.0%, with relative standard deviations (RSD) were in the range of 1.62%~4.27% (n=6). The method is sensitive, reproducible, accurate and precise, and is suitable for the determination of trace pentachlorophenol and its sodium salt residues in animal-origin foods.
Publication Date
7-28-2019
First Page
80
Last Page
86
DOI
10.13652/j.issn.1003-5788.2019.07.014
Recommended Citation
Yanhong, CHEN; Sui, CHEN; Anhua, SONG; Jingchu, HUANG; Yueming, CHEN; Jia, LIU; and Yu, WANG
(2019)
"Establishment of trace pentachlorophenol and its sodium salt in animal-origin foods by automated solid phase extraction-coupled with ultra performance liquid chromatography-tandem mass spectrometry,"
Food and Machinery: Vol. 35:
Iss.
7, Article 14.
DOI: 10.13652/j.issn.1003-5788.2019.07.014
Available at:
https://www.ifoodmm.cn/journal/vol35/iss7/14
References
[1] 杨淑贞, 韩晓冬, 陈伟, 等. 五氯酚对生物体的毒性研究进展[J]. 环境与健康杂质, 2005, 22(5): 396-398.
[2] World Health Organization. IPCS international programme on chemical safety: Health and safety guide N0.19, pentachlorophenol . (2014-05-25) [2019-03-28]. http://www.inchem.org/documents/hsg/hsg/hsg019.htm.
[3] 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.
[4] 梁倩, 朱晓华, 吴光红. 五氯苯酚及其钠盐在渔业产品中的残留与检测方法的研究进展[J]. 中国渔业质量与标准, 2012, 2(1): 71-75.
[5] 农业部. 中华人民共和国农业部公告第193号. (2002-04-09) [2019-03-28]. http://jiuban.moa.gov.cn/zwllm/tzgg/gg/201104/t20110422_1976324.htm.
[6] 农业部. 中华人民共和国农业部公告第235号. (2002-12-24) [2019-03-28]. http://jiuban.moa.gov.cn/zwllm/tzgg/gg/200302/t20030226_59300.htm.
[7] 国家食品药品监督管理局. 国家食品安全监督抽检实施细则: 2018年版 . (2018-01-24) [2019-03-28]. http://samr.cfda.gov.cn/WS01/CL1605/223270.html.
[8] 杭学宇, 冯晓青, 汪怡, 等. 气相色谱法测定小龙虾中五氯酚[J]. 现代预防医学, 2014, 41(5): 803-805.
[9] 唐宏兵, 欧阳运富. 固相微萃取—气相色谱法测定鱼肉中五氯酚[J]. 理化检验: 化学分册, 2011, 47(9): 1 026-1 028.
[10] 张博, 梅勇, 邹晓雪, 等. 顶空固相微萃取—气相色谱法测定尿中五氯酚[J]. 环境与职业医学, 2016, 33(12): 1 187-1 190.
[11] 史玉坤, 杨梅佳, 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] 雍宗锋, 曹慧, 蔡丹丹. 全自动固相萃取—内标衍生—气相色谱—串联质谱法测定肉中五氯酚[J]. 江苏预防医学, 2017, 28(6): 619-621, 625.
[13] 朱晓华, 梁倩, 王凯, 等. 气相色谱—负化学源质谱法测定河蟹中五氯苯酚及其钠盐的残留量[J]. 食品安全质量检测学报, 2016, 7(9): 3 650-3 655.
[14] 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.
[15] 牛增元, 包艳, 叶曦雯, 等. 高效液相色谱法测定木材及其制品中的酚类防腐剂[J]. 分析试验室, 2009, 28(6): 57-60.
[16] 欧天成, 郭艳芬, 陈少芬, 等. 高效液相色谱法同时测定水中挥发性酚(以苯酚计)、2,4,6-三氯酚、五氯酚[J]. 中国卫生工程学, 2018, 17(1): 55-57.
[17] 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.
[18] 李淑红, 赵仕沛, 李迎芳. 直接进样超高效液相色谱—串联质谱法测定水中五氯酚[J]. 河南科学, 2014, 32(2): 169-171.
[19] 闵剑青, 陈梅兰, 陈晓红, 等. 离子液体超声辅助萃取-LC/MS法测定环境水中痕量五氯酚[J]. 分析测试学报, 2015, 34(4): 438-442.
[20] 余宇燕, 张淑玲, 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, 2014, 33(7): 830-834.
[21] 潘胜东, 陈晓红, 何仟, 等. 超高效液相色谱—高分辨质谱确证分析泥鳅体内五氯酚代谢物[J]. 色谱, 2017, 35(12): 1 245-1 250.
[22] JIN Mi-cong, CHEN Xiao-hong, PAN Bing-xian. Simultaneous determination of 19 chloropheols in water by liquid chromatography-mass spectrome-try with solid-phase extraction[J]. Journal of Liquid Chromatography & Related, 2006, 29(9): 1 369-1 380.
[23] 2002/657/EC. Commission decision of 12 August 2002 implementing council directive 96/23/EC concerning the performance of analytical methods and the interpretation of results[S]. [S.l.]: Official Journal of the European Communities, 2002.
[24] 张盼, 苏福海, 戴新华, 等. 棉类纺织品中痕量五氯酚的液相色谱—同位素稀释质谱法测定及不确定度评定[J]. 分析测试学报, 2010, 29(9): 953-957.
[25] GONZLEZ Oskar, BLANCO María-Encarnación, IRIARTE Gorka, et al. Bioanalytical chromatographic method validation according to current regulations, with a special focus on the non-well defined parameters limit of quantification, robustness and matrix effect[J]. Journal of Chromatography A, 2014, 1 353: 10-27.