Chemical Analysis & Physical Testing Institute, Shenzhen Center for Disease Control and Prevention, Shenzhen, China.
Shenzhen Center for Chronic Disease Control, Shenzhen, China.
Sci Prog. 2024 Oct-Dec;107(4):368504241300638. doi: 10.1177/00368504241300638.
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.
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.
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.
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.
本研究旨在开发和验证一种自动化固相萃取(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酚钠(PCP-Na)残留。鉴于 PCP-Na 的潜在危害和环境持久性,开发一种灵敏可靠的方法对于监测食品接触材料中 PCP-Na 的残留至关重要,以确保消费者安全。
采用 10%甲醇水溶液提取砧板木屑,然后使用自动化 SPE 系统进行净化。洗脱液浓缩后,用 UPLC-MS/MS 进行分析。采用同位素标记的内标来减轻基质效应,提高检测灵敏度。通过评估线性度、检测限(LOD)、定量限(LOQ)、回收率和不同浓度水平下的相对标准偏差(RSD)来验证该方法。
该方法在 0 至 100μg/L 的浓度范围内表现出优异的线性关系,回归方程为 Y=1.035X-0.7771,R²为 0.9996。LOD 和 LOQ 分别为 0.4 和 1.0μg/kg。回收率范围为 71.75%至 96.50%,RSD 在 5.19%至 16.66%之间。将该方法应用于 30 个市场砧板样品,发现 50%的样品中存在 PCP-Na 残留,浓度范围为 0 至 83990μg/kg。
本研究提出了一种用于检测砧板上 PCP-Na 的强大 UPLC-MS/MS 方法,提高了检测灵敏度并简化了样品制备。在商业样品中高检出率突显了对消费者进行严格监测和监管措施的必要性,以降低暴露风险。