开发和验证用于检测砧板上五氯酚钠残留物的 LC-MS/MS 方法。

IF 2.6 4区 综合性期刊 Q2 MULTIDISCIPLINARY SCIENCES Science Progress Pub Date : 2024-10-01 DOI:10.1177/00368504241300638
Shicheng Liao, Wanna Xu, Jie Jiang, Honghe Liu, Zhuoying Zeng
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引用次数: 0

摘要

研究目的本研究旨在开发并验证一种自动固相萃取(SPE)与超高效液相色谱-串联质谱(UPLC-MS/MS)联用的方法,用于检测砧板上的五氯苯酚钠(PCP-Na)残留量。鉴于五氯酚钠的潜在危害和环境持久性,灵敏可靠的方法对于监测其在食品接触材料中的残留量以确保消费者安全至关重要:方法:使用 10% 甲醇水溶液萃取砧板上的木屑,然后使用自动 SPE 系统进行净化。对洗脱液进行浓缩、重组,并通过 UPLC-MS/MS 进行分析。使用同位素标记的内标来减轻基质效应,提高检测灵敏度。通过评估不同浓度水平的线性关系、检测限 (LOD)、定量限 (LOQ)、回收率和相对标准偏差 (RSD),对该方法进行了验证:该方法在 0 至 100 μg/L 的浓度范围内表现出良好的线性关系,回归方程为 Y = 1.035X-0.7771,R²为 0.9996。检测限和最低检测限分别为 0.4 和 1.0 μg/kg。回收率为 71.75% 至 96.50%,RSD 为 5.19% 至 16.66%。在 30 份市场砧板样品中,50% 的样品检测到了五氯苯酚-Na 残留,浓度范围为 0 至 83,990 微克/千克:本研究提出了一种检测砧板上五氯苯酚-Na 的高效 UPLC-MS/MS 方法,不仅提高了灵敏度,还简化了样品制备过程。商业样品中的高检出率突出表明,有必要采取严格的监测和监管措施来降低消费者接触五氯苯酚的风险。
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Development and validation of an LC-MS/MS method for the detection of sodium pentachlorophenolate residues on cutting boards.

Objectives: The objective of this study was to develop and validate an automated solid-phase extraction (SPE) coupled with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the detection of sodium pentachlorophenolate (PCP-Na) residues on cutting boards. Given the potential hazards and environmental persistence of PCP-Na, a sensitive and reliable method is crucial for monitoring its residues in food contact materials to ensure consumer safety.

Methods: Wood shavings from cutting boards were extracted using 10% methanol in water, followed by purification using an automated SPE system. The eluent was concentrated, reconstituted, and analyzed by UPLC-MS/MS. An isotope-labeled internal standard was used to mitigate matrix effects, enhancing detection sensitivity. The method was validated by assessing linearity, limit of detection (LOD), limit of quantification (LOQ), recovery rates, and relative standard deviations (RSDs) across various concentration levels.

Results: The method demonstrated excellent linearity over a concentration range of 0 to 100 μg/L with a regression equation of Y = 1.035X-0.7771 and an R² of 0.9996. The LOD and LOQ were determined to be 0.4 and 1.0 μg/kg, respectively. Recovery rates ranged from 71.75% to 96.50% with RSDs between 5.19% and 16.66%. When applied to 30 market cutting board samples, PCP-Na residues were detected in 50% of the samples, with concentrations ranging from 0 to 83,990 µg/kg.

Conclusion: This study presents a robust UPLC-MS/MS method for the detection of PCP-Na on cutting boards, offering improved sensitivity and simplified sample preparation. The high detection rate in commercial samples underscores the need for stringent monitoring and regulatory measures to mitigate the exposure risk to consumers.

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来源期刊
Science Progress
Science Progress Multidisciplinary-Multidisciplinary
CiteScore
3.80
自引率
0.00%
发文量
119
期刊介绍: Science Progress has for over 100 years been a highly regarded review publication in science, technology and medicine. Its objective is to excite the readers'' interest in areas with which they may not be fully familiar but which could facilitate their interest, or even activity, in a cognate field.
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