[固相萃取-超快速液相色谱-串联质谱法测定食品中的五氯苯酚]
[Determination of pentachlorophenol in food by solid phase extraction-ultrafast liquid chromatography-tandem mass spectrometry].
作者信息
Chen Xiaohong, Pan Shengdong, Jin Micong
机构信息
Zhejiang Provincial Key Laboratory of Health Risk Appraisal for Trace Toxic Chemicals, Ningbo Key Laboratory of Poison Research and Control, Ningbo Municipal Center for Disease Control and Prevention, Ningbo 315010, China.
出版信息
Wei Sheng Yan Jiu. 2018 May;47(3):440-458.
OBJECTIVE
A method was developed for the determination of pentachlorophenol( PCP) in food by ultrafast liquid chromatography-tandem mass spectrometry after solid phase extraction.
METHODS
The sample was extracted in 8%triethylamine/acetonitrile( 70/30, V/V) and purified on a MAX-SPE cartridge. The UFLC separation was performed on a Shim-pack XR-ODS Ⅲ column( 150 mm × 2. 0 mm, 2. 2μm) with a linear gradient elution program of acetonitrile and 5 mmol/L ammonium acetate( 0. 1% formic acid) as the mobile phase. Electrospray ionization was applied and operated in the negative ion mode.
RESULTS
The limit of quantitation( LOQ) and limit of detection( LOD) for PCP were 0. 4-0. 5 μg/kg and 0. 12-0. 15 μg/kg. The calibration curve showed good linearity between 0. 5-50. 0 μg/L, and the correlative coefficients( r) were more than 0. 999. The recovery was between 82. 0%-108. 0%, and the RSD was between 1. 89%-5. 09%( n = 6).
CONCLUSION
The method is sensitive, reproducible, and adapts to determination of PCP in variety of foods.
目的
建立一种固相萃取后超快速液相色谱 - 串联质谱法测定食品中五氯酚（PCP）的方法。
方法
样品用8%三乙胺/乙腈（70/30，V/V）提取，并在MAX - SPE柱上纯化。超快速液相色谱分离在Shim - pack XR - ODSⅢ柱（150 mm×2.0 mm，2.2μm）上进行，以乙腈和5 mmol/L醋酸铵（0.1%甲酸）作为流动相，采用线性梯度洗脱程序。采用电喷雾电离，在负离子模式下运行。
结果
PCP的定量限（LOQ）和检测限（LOD）分别为0.4 - 0.5μg/kg和0.12 - 0.15μg/kg。校准曲线在0.5 - 50.0μg/L之间呈良好线性，相关系数（r）大于0.999。回收率在82.0% - 108.0%之间，相对标准偏差（RSD）在1.89% - 5.09%之间（n = 6）。
结论
该方法灵敏、可重现，适用于多种食品中PCP的测定。
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