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固相萃取-液相色谱/电喷雾串联质谱法测定主流烟气中的吡啶、2-吡啶、4-吡啶和喹啉。

Determination of pyridine, 2-picoline, 4-picoline and quinoline from mainstream cigarette smoke by solid-phase extraction liquid chromatography/electrospray ionization tandem mass spectrometry.

机构信息

Department of Chemistry, Jadavpur University, Kolkata 700032, West Bengal, India.

出版信息

J Chromatogr A. 2010 Jan 15;1217(3):307-11. doi: 10.1016/j.chroma.2009.11.050. Epub 2009 Nov 24.

Abstract

The present paper describes the development and validation of a new reversed-phase liquid chromatography-electrospray ionization tandem mass spectrometric method (RP-HPLC-ESI-MS/MS) for simultaneous determination of pyridine, 2-picoline, 4-picoline and quinoline from mainstream cigarette smoke. Liquid-liquid extraction followed by solid-phase extraction was applied to extract the target analytes from cigarette smoke. Baseline chromatographic separation was achieved by utilizing a Zorbax SB-Aq (4.6x150 mm, 5 microm) column in gradient chromatographic conditions with acetonitrile and ammonium acetate buffer as mobile phases. Popular commercially available Indian brand filtered and non-filtered cigarettes were analyzed using the same method. The identification of each chemical was established by chromatographic retention times, analyte specific fragmentation patterns and relative peak area ratios of two product/precursor ion pairs. The limit of detection of this method ranged from 1.74 to 14.32 ng/cig using an injection volume of 20 microl. The reproducibility of this method is excellent and better standard deviations were obtained compared to literature reported values for these chemicals. RSD value is less than 9% for all analytes.

摘要

本研究建立了一种同时测定主流烟气中吡啶、2-皮考啉、4-皮考啉和喹啉的反相高效液相色谱-电喷雾串联质谱法(RP-HPLC-ESI-MS/MS)。采用液液萃取-固相萃取法提取香烟中的目标分析物。在梯度洗脱条件下,使用 Zorbax SB-Aq(4.6x150mm,5μm)色谱柱进行基线分离,以乙腈和乙酸铵缓冲液为流动相。采用相同的方法分析了流行的印度品牌过滤和非过滤香烟。通过色谱保留时间、特定的分析物碎片模式和两个产物/前体离子对的相对峰面积比来确定每种化学物质的鉴定。该方法的检出限为 1.74-14.32ng/cig,进样量为 20μl。与文献报道的这些化学物质相比,该方法具有良好的重现性,得到了更好的标准偏差。所有分析物的 RSD 值均小于 9%。

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