超高效液相色谱-三重四极杆质谱法快速测定煎炸过程用油中的苯并a芘
Rapid Determination of BenzoaPyrene in Deep Frying Oil by Ultra Performance Liquid Chromatography-triple Quadrupole Mass Spectrometry
-
摘要: 建立快速检测煎炸过程用油中苯并a芘的超高效液相色谱-三重四极杆质谱联用(UPLC-MS/MS)分析方法。样品用乙腈提取后,经EMR-Lipid脂质增强型固相萃取柱净化,以乙腈和水作为流动相进行梯度洗脱,在RRHD SB-C18柱上实现分离,大气压化学电离(APCI)-三重四极杆质谱正离子多反应监测(MRM+)方式检测,以苯并a芘-d12作为内标的稳定同位素稀释法定量。结果表明,方法的线性范围为1~200 μg/kg,决定系数R2=0.9997,检出限为0.2 μg/kg,定量限为0.6 μg/kg。平均加标回收率为94.0%~98.7%,相对标准偏差为2.1%~5.6%。20批样品中均检出苯并a芘,含量在1.76~6.81 μg/kg之间。该方法前处理简单、基质干扰少、定性定量准确、灵敏度高,适用于煎炸过程用油中苯并a芘的测定。Abstract: A method for the determination of benzoapyrene in deep frying oil was developed by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Samples were extracted with acetonitrile and purified by EMR-Lipid SPE column. The separation of benzoapyrene was carried out on a RRHD SB-C18 column with gradient elution of acetonitrile and water. An atmospheric pressure chemical ionization (APCI) interface was used as the ion source and the analysis was performed in the multiple reaction monitoring (MRM) mode, the samples were quantified by isotope dilution mass spectrometry (IDMS) with benzoapyrene-d12 as internal standard. The results of method showed the linearity in the range of 1~200 μg/kg, R2=0.9997.The limit of detection (LOD) was 0.2 μg/kg and the limits of quantification (LOQ) was 0.6 μg/kg. The average recovery ranged from 94.0% to 98.7% with the relative standard deviation (RSD) range of 2.1%~5.6%. Benzoapyrene was detected in the 20 samples, and the content was 1.76~6.81 μg/kg. The results suggested the method was suitable for the detection of benzoapyrene in deep frying oil, for its obvious advantages such as simpler pretreatment, higher accuracy and sensitivity.