超高效液相色谱法同时测定烟用香精料液中的糠醛、5-羟甲基糠醛与5-甲基糠醛

Simultaneous Determination of Furfural,5-Hydroxymethylfurfural and 5-Methylfurfural in Cigarette Fragrances by Ultra-high Performance Liquid Chromatography

建立了同时测定烟用香精料液中糠醛、5-羟甲基糠醛和5-甲基糠醛的超高效液相色谱（UPLC）方法。样品经流动相稀释、振荡、过滤后,采用C18（2.1 mm i.d.×100 mm,1.7μm）柱,以乙腈-水（10∶90）为流动相,在流速0.3 m L/min条件下等度洗脱分离,以二极管阵列检测器在波长280 nm下检测,外标法定量。该方法5 min内即可实现3种目标物的分离,5-羟甲基糠醛、糠醛和5-甲基糠醛的线性范围分别为0.004 2~40.00 mg/kg,0.004 6~30.00 mg/kg,0.006 9~30.00 mg/kg;相关系数（r2）分别为0.999 2,0.999 9和0.999 8;检出限（S/N=3）分别为1.24,1.37,2.06μg/kg;相对标准偏差（RSD,n=11）为0.1%~0.4%;加标水平为0.005 0~10.18 mg/kg时,3种化合物的回收率为91.7%~106.0%。该方法操作简便、分析快速、结果准确,适用于烟用香精料液中5-羟甲基糠醛、糠醛和5-甲基糠醛的检测。

An ultra-high performance liquid chromatographic（ UPLC） method for the simultaneous determination of furfural,5-hydroxymethylfurfural and 5-methylfurfural in cigarette fragrances was established. After dilution,vibration and filtration,the cigarette additives were separated on a C18（ 2. 1mm i. d. × 100 mm,1. 7 μm） column under isocratic elution mode using acetonitrile- water（ 10 ∶90） as mobile phase at a flow rate of 0. 3 m L / min. The quantification of these analytes was achieved by the external standard method with a diode-array detector at 280 nm. Baseline separation of these analytes was achieved within 5. 0 min. The linear ranges for 5-hydroxymethylfurfural,furfural and 5-methylfurfural were in the ranges of 0. 004 2- 40. 00 mg / kg,0. 004 6- 30. 00 mg / kg,0. 006 9-30. 00 mg / kg,with correlation coefficients（ r2） of 0. 999 2,0. 999 9 and 0. 999 8,respectively.The detection limits（ S / N = 3） for three analytes were 1. 24,1. 37,2. 06 μg / kg, respectively.Relative standard deviations（ RSD,n = 11） were in the range of 0. 1%- 0. 4%. The recoveries at spiked concentration of 0. 005 0- 10. 18 mg / kg were 91. 7%- 106. 0%. The proposed method has the merits of easy operation,fast analysis and accurate results,and is suitable for the simultaneous determination of 5-hydroxymethylfurfural,furfural and 5-methylfurfural in cigarette fragrances.