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
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(丽水市疾病预防控制中心,浙江 丽水 323000)

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李启 女 副主任技师 研究方向为理化检验 E-mail:liky3524@126.com

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Determination of sodium pentachlorophenolate in chopping board by liquid liquid extraction-ultra performance liquid chromatography-tandem mass spectrometry
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(Lishui Center for Disease Prevention and Control, Zhejiang Lishui 323000, China)

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    摘要:

    目的 建立一种适用于测定砧板中五氯酚钠的液液萃取-超高效液相色谱-串联质谱方法。方法 样品采用50%甲醇水溶液(含1%氨水)萃取,超声提取10 min后,用正己烷-二氯甲烷(8∶2,V/V)萃取,氮吹近干,以0.01%氨水和甲醇溶液复溶后进行超高效液相分离,在电喷雾离子源负离子(ESI-)多反应监测(MRM)模式下进行质谱检测。结果 本方法的检出限为0.2 μg/kg,在1、4和20 μg/kg三个加标水平下的回收率为101.4%~108.9%,相对标准偏差为3.5%~7.8%(n=7)。应用该方法检测市售60份砧板,其中1份样品检出五氯酚钠残留,含量为1.16 μg/kg。结论 本方法简便、高效,适用于砧板中痕量五氯酚钠的快速测定,结果准确可靠。

    Abstract:

    Objective A new liquid liquid extraction-ultra performance liquid chromatography-tandem mass spectrometry method was developed for the determination of sodium pentachlorophenolate in chopping board. Methods Samples were ultrasonic extracted with 50% methanol/aqueous solution(1% ammonia)for 10 min, followed by extraction with n-hexane-dichloromethane(8∶2,V/V). Then the analyte was evaporated to dryness and dissolved with 0.01% ammonia-methanol. After being ultra performance separated on a column using mobile phase, the analytes were detected under electrospray source negative ion (ESI-) multi reaction monitoring (MRM) mode by tandem mass spectrometry. Results The limit of detection for sodium pentachlorophenolate was 0.2 μg/kg. The result showed that the average recovery at spiking level of 1,4,20 μg/kg ranged from 101.4% to 108.9% and the relative standard deviation was 3.5%-7.8% (n=7).The method had been successfully applied to the measurement of sodium pentachlorophenolate in 60 chopping board samples shopped from Lishui markets, and one of the samples had sodium pentachlorophenolate with 1.16 μg/kg . Conclusion The liquid liquid extraction method is easy, economic and efficient. The ultra performance liquid chromatography-tandem mass spectrometry method is rapid and accurate to confirmatively detect sodium pentachlorophenolate in chopping board.

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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.

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  • 收稿日期:2019-04-19
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  • 在线发布日期: 2019-07-09
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