基于棒状核-壳结构的磁性沸石咪唑酯骨架复合材料的磁固相萃取-气相色谱-质谱法检测茶饮料中16种多环芳烃OA北大核心CSTPCD
Determination of Sixteen Kinds of Polycyclic Aromatic Hydrocarbons in Tea Beverages by MHNTs@ZIF-8-based Magnetic Solid Phase Extraction-Gas Chromatography-Mass Spectrometry
制备了具有棒状核-壳结构的磁性沸石咪唑酯骨架复合材料(MHNTs@PDA@ZIF-8),并将其作为磁固相萃取(MSPE)的吸附剂,结合气相色谱-质谱联用(GC-MS)技术,建立了一种测定茶饮料中16种多环芳烃(PAHs)的方法.采用扫描电子显微镜(SEM)、傅里叶红外光谱(FT-IR)、X射线衍射仪(XRD)、振动样品磁强计(VSM)和氮气吸附-脱附实验对此复合材料进行了表征,结果表明,制备的MHNTs@PDA@ZIF-8吸附剂具有较强的磁性和较大的比表面积.考察了吸附剂用量、萃取时间和解吸时间等因素对萃取效率的影响,得到最佳萃取条件为:以10 mg MHNTs@PDA@ZIF-8作为吸附剂,涡旋萃取90 s,1 mL正己烷超声解吸60 s.本方法对16种PAHs在5~500 μg/L范围内具有良好的线性关系,相关系数r2≥0.995,检出限(S/N=3)为0.1~0.8 μg/L,定量限(S/N=10)为0.3~2.6 μg/L,加标回收率为60.9%~114.7%,相对标准偏差(RSD)为0.2%~9.2%.本方法操作简单、萃取时间短、灵敏度高、样品和有机溶剂消耗少,适用于茶饮料中16种PAHs的同时检测.
MHNTs@PDA@ZIF-8 with rod-shaped core-shell structures was synthesized and used as sorbent in magnetic solid phase extraction(MSPE).MHNTs@PDA@ZIF-8-MSPE method coupled with gas chromatography-mass spectrometry(GC-MS)was employed to analyze sixteen kinds of polycyclic aromatic hydrocarbons(PAHs)in tea beverages.Vibrating sample magnetometer(VSM),Fourier transform infrared spectroscopy(FT-IR),X-ray diffraction(XRD),scanning electron microscopy(SEM)and nitrogen adsorption-desorption techniques were used to characterize the MHNTs@PDA@ZIF-8.The results demonstrated that the MHNTs@PDA@ZIF-8 exhibited significant magnetic properties and a large specific surface area.The experimental conditions that could affect MSPE were investigated,including adsorbent dosage,extraction time,desorption time,ionic strength,desorption solvent type,and desorption solvent volume.The optimal conditions were 10 mg of MHNTs@PDA@ZIF-8 as adsorbent,90 s under vortex extraction,and ultrasonic desorption for 60 s with 1 mL ofn-hexane.The sixteen kinds of PAHs showed good linearity in the concentration range of 5-500 μg/L(r2≥0.995).The limits of detection(S/N=3)and quantitation(S/N=10)were in the range of 0.1-0.8 μg/L and 0.3-2.6 μg/L,respectively.The recoveries of the method ranged from 60.9%to 114.7%,with relative standard deviations(n=3)ranging from 0.2%to 9.2%when the addition levels of sixteen kinds of PAHs were 10,50,and 100 μg/L.The method was simple,fast,sensitive and environmentally friendly,and suitable for detecting sixteen kinds of PAHs in tea beverages.
聂文丁;帅思婕;胡珂;崔晓垒;王静;李东东;李腾飞
河北工程大学生命科学与食品工程学院,邯郸 056038河北省地质矿产勘查开发局第一地质大队实验室,邯郸 056000河北工程大学材料科学与工程学院,邯郸 056038
沸石咪唑酯骨架埃洛石纳米管多环芳烃磁固相萃取茶饮料
Zeolitic imidazolate frameworksHalloysite nanotubesPolycyclic aromatic hydrocarbonsMagnetic solid-phase extractionTea beverages
《分析化学》 2024 (009)
1355-1364,中插36-中插38 / 13
河北省重点研发计划项目(No.22325501D)资助. Supported by the Key Research and Development Project of Hebei Province,China(No.22325501D).
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