ASPE-UPLC-MS/MS测定动物源食品中痕量五氯酚及其钠盐
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(1. 广州市食品检验所,广东 广州 511400;2. 广东美味鲜调味食品有限公司,广东 中山 528437)

作者简介:

陈彦宏,女,广州市食品检验所助理工程师。

通讯作者:

王宇(1980—),男,广州市食品检验所高级工程师,博士。E-mail:94180681@qq.com

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基金项目:

广东省科技计划项目(编号:2016A040403077);广州市科技计划项目(编号:201804010403);广东美味鲜博士后科技创新项目(编号:2018)


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
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(1. Guangzhou Institute For Food Inspection, Guangzhou, Guangdong 511400, China; 2. Guangdong Meiweixian Flavoring Foods Co., Ltd., Zhongshan, Guangdong 528437, China)

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    摘要:

    建立了全自动固相萃取—超高效液相色谱—串联质谱法测定动物源食品中五氯酚及其钠盐的分析方法,比较了提取溶剂、固相萃取柱、洗脱液、质谱分析和色谱分离条件、内标物等对测定结果的影响。最终选用5%氨水—乙腈提取,MAX固相萃取柱净化,10%甲酸甲醇溶液洗脱,氮吹浓缩后用乙腈—水溶液(5050,体积比)定容,Kinetex C18色谱柱(100 mm×2.1 mm,2.6 μm)分离,乙腈和5 mmol/L乙酸铵的0.1%甲酸水溶液梯度洗脱,电喷雾电离负离子(ESI-)多反应监测模式(MRM)检测,内标法定量。结果显示:五氯酚在0.2~10.0 μg/L 范围内线性关系良好,相关系数r>0.999;1.0,5.0,10.0 μg/kg添加水平下的加标回收率在86.0%~106.0%,相对标准偏差(RSD)为1.62%~4.27%。该方法灵敏度高,重现性好,具有较高的准确度和精密度,可用于测定动物源食品中痕量五氯酚及其钠盐残留。

    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.

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陈彦宏,陈穗,宋安华,等. ASPE-UPLC-MS/MS测定动物源食品中痕量五氯酚及其钠盐[J].食品与机械,2019,(7):80-86.
CHENYanhong, CHENSui, SONGAnhua, et al. 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[J]. Food & Machinery,2019,(7):80-86.

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  • 收稿日期:2019-03-01
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  • 在线发布日期: 2022-11-25
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