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Determination of basic azaarenes in aviation kerosene by solid-phase extraction and HPLC-fluorescence detection

机译:固相萃取-高效液相色谱-荧光检测法测定航空煤油中的碱性氮杂

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摘要

SPE in combination with HPLC and fluorescence detection has been used for sensitive determination of six basic azaarenes (7,8-benzoquinoline, 7,9-dimethylbenz[c]-acridine, 9-amino-1,2,3,4-tetrahydroacridine, 9-methylacridine, acridine, and dibenz[a,j]acridine) in aviation kerosene (jet fuel). SPE was performed in a single step using a strong cation exchange sorbent. The HPLC system consisted of C18 column with a selected detection program of optimal lambda(exc) and lambda(em). A gradient elution with ACN and phosphate buffer (pH 6.5) at a flow rate of 1 mL/min allowed efficient and fast separation of azaarenes within 15 min. The LOD and LOQ values (S/N ratio 3:1 and 10:1, respectively) were between 0.0013 and 0.021 and from 0.0044 to 0.072 ng per injection. The calibration curves showed linear behavior from the LOQ to 250 mu g/L (r(2) > 0.99). For the spiked concentration of 6.0 mu g/L, recoveries were from 92 to 107% for jet fuel samples, except for 9-amino-1,2,3,4-tetrahydroacridine, which presented 68% recovery. The proposed method was applied to the quantification of those six basic azaarenes in one commercial kerosene and in three aviation kerosene samples. The presence of 7,8-benzoquinoline (up to 3.2 mu g/L) and dibenzo[a,j]acridine (up to 6.3 mu g/L) was confirmed in aviation kerosene.
机译:SPE与HPLC和荧光检测相结合已用于灵敏测定6种碱性氮杂氮杂(7,8-苯并喹啉,7,9-二甲基苯并[c] -ac啶,9-氨基-1,2,3,4-四氢ac啶,航空煤油(喷气燃料)中的9-甲基ac啶,a啶和二苯并[a,j] ac啶。使用强阳离子交换吸附剂,只需一步即可完成SPE。 HPLC系统由具有最佳lambda(exc)和lambda(em)选定检测程序的C18色谱柱组成。用ACN和磷酸盐缓冲液(pH 6.5)以1 mL / min的流速进行梯度洗脱,可以在15分钟内高效,快速地分离氮杂芳烃。 LOD和LOQ值(信噪比分别为3:1和10:1)在0.0013和0.021之间,每次注射从0.0044到0.072 ng。校准曲线显示了从LOQ到250μg / L的线性行为(r(2)> 0.99)。对于6.0μg / L的加标浓度,航空燃油样品的回收率为92%至107%,但9-氨基-1,2,3,4-四氢ac啶的回收率为68%。所提出的方法用于一种商业煤油和三种航空煤油样品中这六个碱性氮杂芳烃的定量分析。航空煤油中证实存在7,8-苯并喹啉(最高3.2微克/升)和二苯并[a,j] r啶(最高6.3微克/升)。

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