Wang Ye, Hu Mingyou, Wang Fang, Yu Juan, Shao Guojian
Huzhou Center for Disease Control and Prevention, Key Laboratory of Emergency Detection for Public Health of Huzhou, Huzhou, China.
PLoS One. 2025 Jun 16;20(6):e0326129. doi: 10.1371/journal.pone.0326129. eCollection 2025.
Sodium pentachlorophenate (PCP-Na) is a toxic preservative used in wood products, posing potential health risks through food contact materials. A rapid analytical method combining ultrasonic-assisted liquid-liquid extraction with ultra-performance liquid chromatography-high resolution mass spectrometry (UA-LLE-UPLC-HRMS) was developed for the determination of PCP-Na residues in bamboo and wooden cutting boards. Sample pretreatment involved ultrasonic extraction using methanol/water (50:50 v/v, 2.0% ammonia), followed by liquid-liquid purification with n-hexane/ethyl acetate (60:40 v/v). After solvent evaporation under nitrogen, the residue was reconstituted in the initial mobile phase. Chromatographic separation was achieved on an Acquity UPLC BEH C18 column (2.1 mm × 100 mm, 1.7 µm) using a gradient elution of methanol and 0.01% ammoniated aqueous solution. Detection was performed in negative electrospray ionization (ESI-) mode with targeted single ion monitoring (Targeted-SIM) scanning, utilizing pentachlorophenol-13C6 (PCP-13C6) as an isotopically labeled internal standard. The method exhibited excellent linearity across a concentration range of 1.0-500.0 μg/L (R2 ≥ 0.999), with a limit of detection (LOD) of 0.5 μg/kg and a limit of quantification (LOQ) of 1.5 μg/kg. Validation studies at three spiking levels (20.0, 200.0, and 400.0 μg/kg) demonstrated satisfactory recoveries of 97.2%-99.7% and precision with relative standard deviations (RSDs) of 0.8%-1.7% (n = 6). The total chromatographic runtime was optimized to 6 minutes. Application of this method to Seventy-five commercial cutting boards revealed PCP-Na residues in five samples, with concentrations ranging from 1.3 to 416 mg/kg. This approach features streamlined sample preparation, high sensitivity, robust accuracy, and rapid analysis, making it particularly suitable for routine monitoring of PCP-Na residues in bamboo and wooden food contact materials.
五氯酚钠（PCP-Na）是一种用于木制品的有毒防腐剂，可通过食品接触材料带来潜在健康风险。本文开发了一种将超声辅助液液萃取与超高效液相色谱-高分辨率质谱联用（UA-LLE-UPLC-HRMS）的快速分析方法，用于测定竹制和木制砧板中PCP-Na的残留量。样品预处理包括使用甲醇/水（50:50 v/v，含2.0%氨水）进行超声萃取，然后用正己烷/乙酸乙酯（60:40 v/v）进行液液净化。氮气吹干溶剂后，残留物用初始流动相复溶。采用Acquity UPLC BEH C18色谱柱（2.1 mm×100 mm，1.7 µm），以甲醇和0.01%氨水溶液进行梯度洗脱实现色谱分离。采用负离子电喷雾电离（ESI-）模式，以五氯酚-13C6（PCP-13C6）作为同位素标记内标进行靶向单离子监测（Targeted-SIM）扫描检测。该方法在1.0 - 500.0 μg/L浓度范围内具有良好的线性（R2≥0.999），检出限（LOD）为0.5 μg/kg，定量限（LOQ）为1.5 μg/kg。在三个加标水平（20.0、200.0和400.0 μg/kg）下进行的验证研究表明，回收率为97.2% - 99.7%，精密度良好，相对标准偏差（RSD）为0.8% - 1.7%（n = 6）。总色谱运行时间优化至6分钟。将该方法应用于75个市售砧板，发现5个样品中存在PCP-Na残留，浓度范围为1.3至416 mg/kg。该方法具有样品制备流程简便、灵敏度高、准确性好和分析速度快等特点，特别适用于竹制和木制食品接触材料中PCP-Na残留的常规监测。
