1.中国人民公安大学 侦查学院,北京 100038
2.东南大学 化学化工学院,江苏 南京 211189
3.南京市公安局刑事科学技术研究所,江苏 南京 210001
杨瑞琴,博士,教授,研究方向:法庭化学,E-mail:yangruiqin@ppsuc.edu.cn
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卢思佳,杨瑞琴,于素华等.离心超滤/离子色谱-三重四极杆质谱法同时测定蔬菜中乙烯利和2,4-二氯苯氧乙酸[J].分析测试学报,2022,41(02):261-265.
LU Si-jia,YANG Rui-qin,YU Su-hua,et al.Simultaneous Determination of Ethephon and 2,4-Dichlorophenoxy-Acetic Acid in Vegetables by Centrifugal Ultrafiltration/Ion Chromatography- Triple Quadrupole Mass Spectrometry[J].Journal of Instrumental Analysis,2022,41(02):261-265.
卢思佳,杨瑞琴,于素华等.离心超滤/离子色谱-三重四极杆质谱法同时测定蔬菜中乙烯利和2,4-二氯苯氧乙酸[J].分析测试学报,2022,41(02):261-265. DOI: 10.19969/j.fxcsxb.21062801.
LU Si-jia,YANG Rui-qin,YU Su-hua,et al.Simultaneous Determination of Ethephon and 2,4-Dichlorophenoxy-Acetic Acid in Vegetables by Centrifugal Ultrafiltration/Ion Chromatography- Triple Quadrupole Mass Spectrometry[J].Journal of Instrumental Analysis,2022,41(02):261-265. DOI: 10.19969/j.fxcsxb.21062801.
建立了离心超滤净化,离子色谱-串联三重四极杆质谱(IC-MS)同时测定蔬菜中乙烯利和2,4-二氯苯氧乙酸(2,4-D)的分析方法。茄子、番茄、玉米和辣椒4种蔬菜经均质机打浆,依次经离心超滤和0.22 μm的无机针筒过滤器净化后,进入IonPac AS19离子色谱柱分离,采用60.0 mmol/L的KOH溶液等度淋洗,流出液经阴离子抑制器抑制后进入质谱,负离子模式下采用多离子监测方式检测,外标法定量。结果表明,当乙烯利和2,4-D的质量浓度在0.5~200.0 μg/L范围内时线性关系良好(,r, ≥ 0.999 5),乙烯利和2,4-D的检出限分别为0.2 μg/L和0.05 μg/L,定量下限分别为0.7 μg/L和0.17 μg/L。乙烯利和2,4-D在4种蔬菜中的平均回收率分别为88.3%~96.8%、92.5%~102%,日内相对标准偏差(intra-RSD,,n, = 6)分别为2.6%~5.9%、1.2%~4.4%,日间相对标准偏差(inter-RSD,,n, = 6)分别为2.2%~5.4%、1.1%~3.4%。利用该方法测定4份市售蔬菜,均检出两种待测物,其中乙烯利的含量为17.5~412.6 μg/kg,2,4-D的含量为1.1~4.1 μg/kg。该方法能满足蔬菜中乙烯利和2,4-D的同时检测,并为公安实战中食品安全案件的检验提供了参考。
A method based on centrifugal ultrafiltration combing with ion chromatography-triple quadrupole mass spectrometry(IC-MS) was established for the simultaneous determination of ethephon and 2,4-dichlorophenoxy-acetic acid(2,4-D) in vegetables.Four vegetables,i.e eggplant,tomato,corn and chili were pulped with a homogenizer.The samples were purified by centrifugal ultrafiltration with a 0.22 μm inorganic syringe filter.The separation of ethephon and 2,4-D were carried out on an IonPac AS19 analytical column by isocratic elution with 60.0 mmol/L KOH as mobile phase.After reducing the conductance with an in-line suppressor,the target compounds in the eluent were detected by MS with negative electrospray ionization under multiple reaction monitoring(MRM) mode,and quantified by the external spiked method.The results showed that the calibration curves were linear(,r, ≥ 0.999 5) in the range of 0.5-200.0 μg/L.The limits of detection for ethephon and 2,4-D were 0.2 μg/L and 0.05 μg/L,the limits of quantitation were 0.7 μg/L and 0.17 μg/L,respectively.The average recoveries for ethephon and 2,4-D in four vegetables were in the range of 88.3%-96.8% and 92.5%-102%,with intra-RSDs(,n, = 6) of 2.6%-5.9% and 1.2%-4.4%,and inter-RSDs(,n, = 6) of 2.2%-5.4% and 1.1%-3.4%,respectively.Furthermore,the established method was successfully applied to the determination of the pesticides in 4 vegetable samples purchased from local markets in Nanjing.Both ethephon and 2,4-D were detected with contents of 17.5-412.6 μg/kg and 1.1-4.1 μg/kg,respectively.The results showed that the method could meet the requirements for the simultaneous and rapid determination of ethephon and 2,4-D in vegetables,and provide a guidance for the detection of food safety cases in actual combat of public security.
离心超滤离子色谱-三重四极杆质谱法(IC-MS)蔬菜乙烯利2,4-二氯苯氧乙酸(2,4-D)
centrifugal ultrafiltrationion chromatography-triple quadrupole mass spectrometry(IC-MS)vegetablesethephon2,4-dichlorophenoxy-acetic acid (2,4-D)
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