高效液相色谱-串联质谱法同时测定烟草中5种Amadori化合物

Simultaneous determination of five Amadori compounds in tobacco byhighperformance liquid chromatography-mass spectrometry

建立了高效液相色谱-三重四极杆质谱（HPLC-QqQ MS）联用定量分析烟草中5种Amadori前香物质的方法。样品经含5%（v/v）甲醇的水提取后,采用Waters XBridgeTMAmide色谱柱（250 mm×4.6 mm,3.5μm）、以甲醇-水为流动相进行分离,采用多反应监测（MRM）模式测定烟草样品中5种Amadori化合物的含量。结果表明,5种Amadori化合物的峰面积与质量浓度的线性关系良好,相关系数r为0.989 5~0.998 9;定量限（S/N=10）在10.18~44.58μg/L,检出限（S/N=3）在3.51~14.86μg/L;平均加标回收率为92.6%~123.6%,相对标准偏差（RSD）小于9.4%。本方法操作简便、灵敏度高、分析速度快,可以用于烟叶及卷烟中5种主要Amadori类物质的含量测定。

A method of high performance liquid chromatography-triple quadrupole mass spec- trometry （HPLC-QqQ MS ） in multiple reaction monitoring （MRM） mode for simultaneous determination of five Amadori compounds in tobacco has been developed. The separation was performed on an XBridgeTM Amide column （250 mm x 4.6 mm, 3.5 μm） by gradient elution using methanol and water as mobile phases. The linearity of this method was good with the correlation coefficients （r） of 0. 989 5 - 0. 998 9. The limits of detection （S/N = 3 ） were from 3.51 μg/L to 14.86 μg/L, and the limits of quantitation （ S/N = l0 ） were from 10. 18 μg/L to 44.58μg/L. The recoveries varied from 92.6% to 123.6% with the relative standard deviations （RSDs） less than 9.4%. The established method is rapid, accurate, robust and convenient, and it could be applied to the measurement of the five Amadori compounds in tobacco and ciga- rettes.