超高效液相色谱法同时测定膨胀烟丝中3种糠醛类化合物

Simultaneous Determination of 3 Furfural Compounds in Expanded Cut Tobacco by UHPLC

粉碎后的膨胀烟丝样品(约1g)用乙腈-二氯甲烷(1+1)混合液20 mL超声提取40min,取适量上清液在10 000r·min^(-1)转速下离心15min,过0.22μm的滤膜。采用超高效液相色谱法同时测定滤液中3种糠醛类化合物的含量。以ACCQ-TAG^(TM)ULTRA C_(18)色谱柱为分离柱,以乙腈(1+9)溶液为流动相,在检测波长284nm处进行测定。3种糠醛类化合物的质量浓度在一定范围内与其对应的峰面积呈线性关系,检出限(3s)为0.012～0.015 mg·L^(-1),测定下限(10s)为0.040～0.050mg·L^(-1)。方法用于膨胀烟丝样品的分析,加标回收率为76.1%～102%,测定值的相对标准偏差(n=5)为3.2%～4.9%。

The crushed sample(about 1 g) of expanded tobacco was extracted ultrasonically for 40 min with 20 mL of the mixture of acetonitrile and dichloromethane(1+1).Appropriate supernatant was centrifugated for 15 min at the speed of 10 000 r·min-1 and filtered on 0.22μm membrane.UHPLC was applied to the simultaneous determination of 3 furfural compounds in the filtrate.ACCQ-TAGTMULTRA C18 chromatographic column was used as separation column,and acetonitrile(1+9) solution was used as mobile phase.Detection at 284 nm was adopted in the determination.Linear relationships between values of peak area and mass concentration of the 3 furfural compounds were kept in definite ranges,with detection limits(3s) in the range of 0.012-0.015 mg·L-1 and lower limits of determination(10s) in the range of 0.040-0.050 mg·L-1.The proposed method was applied to the analysis of the sample of expanded cut tobacco,giving values of recovery found by standard addition method and RSDs(n=5) of determined values in the ranges of 76.1%-102% and 3.2%-4.9% respectively.