CAJ | 학술논문

目的：采用高效液相色谱-四级杆/静电场轨道阱高分辨质谱建立分散固相萃取法(dispersive solid phase extraction, d-SPE)快速分析植物油中16种邻苯二甲酸酯(Phthalate esters, PAEs)的检测方法。方法样品采用正己烷饱和的乙腈提取,经N-丙基乙二胺(primary secondary amine, PSA)和Nano Carb填料分散固相萃取净化,以BEH phenyl色谱柱为分析柱,0.1%甲酸乙腈及0.1%甲酸水溶液作为流动相进行梯度洗脱分离。采用正离子采集模式对植物油样品进行快速筛查,并对16种PAEs进行定量测定。结果16种PAEs在2~500μg/L范围内呈良好的线性关系,回归系数(r)大于0.995,该方法的定量限为8~10μg/kg。在不同加标水平下的平均回收率为77.9%~115.6%,相对标准偏差为0.3%~8.9%。结论本方法简单、灵敏、准确,适用于植物油中PAEs的快速筛查和定量测定。
목적：채용고효액상색보-사급간/정전장궤도정고분변질보건립분산고상췌취법(dispersive solid phase extraction, d-SPE)쾌속분석식물유중16충린분이갑산지(Phthalate esters, PAEs)적검측방법。방법양품채용정기완포화적을정제취,경N-병기을이알(primary secondary amine, PSA)화Nano Carb전료분산고상췌취정화,이BEH phenyl색보주위분석주,0.1%갑산을정급0.1%갑산수용액작위류동상진행제도세탈분리。채용정리자채집모식대식물유양품진행쾌속사사,병대16충PAEs진행정량측정。결과16충PAEs재2~500μg/L범위내정량호적선성관계,회귀계수(r)대우0.995,해방법적정량한위8~10μg/kg。재불동가표수평하적평균회수솔위77.9%~115.6%,상대표준편차위0.3%~8.9%。결론본방법간단、령민、준학,괄용우식물유중PAEs적쾌속사사화정량측정。
Objective To establish a dispersive solid phase extraction (d-SPE)/high-resolution benchtop Q exactive mass spectrometry (HRMS) method for the rapid analysis of 16 phthalate esters (PAEs). Methods The samples were extracted with acetonitrile saturated with hexane, and cleaned up by d-SPE with the N-propyl ethlene diamine (PSA) and Nano Carb as the sorbents. The chromatographic analysis was performed on a BEH phenyl column with 0.1%formic acid in acetonitrile and 0.1%formic acid solution as the mobile phase and a gradient elution program was used. The PAEs were analyzed in positive mode by Q exactive high-resolution mass spectrometry, which were applied in rapid analysis of PAEs for vegetable oils. 16 PAEs analytes were screened qualitatively in the vegetable oil samples and then quantified by isotope dilution technique. Results All the target 16 PAEs showed a good linearity in the range of 2~500μg/L , and the aver-age recovery rates of the spiked vegetable oil samples were in the range of 77.9%~115.6%with the RSD in the range of 0.3%-8.9%. The limit of quantification (LOQ) for 16 PAEs in vegetable oil were between 8μg/kg and 10μg/kg. Conclusion The method was simple, sensitive and accurate, and was suitable for the rapid analysis of 16 PAEs in vegetable oils.