高效液相色谱法附蒸发光散射检测器同时测定烟用接装纸中7种甜味剂的含量

Determination of 7 Sweeteners in Cigarette Tip Paper by High Performance Liquid Chromatography with Evaporation Light Scattering Detection

取接装纸样品剪碎成5mm×5mm的小片,称取2.0000g用水20mL摇床振荡萃取35min,所得萃取液经0.22μm滤膜过滤,取其滤液进行高效液相色谱分析,用蒸发光散射检测器检测。选用ZORBAX SB C18色谱柱为固定相,进样量为10μL。用不同比例的(A)甲醇(每升中含三氟乙酸0.1mL,pH 4.5)和(B)水的混合液作为流动相进行梯度洗脱。在此条件下,所测定的7种甜味剂可达到有效的分离。以7种甜味剂所给出的峰面积对其相应的质量浓度绘制标准曲线,其线性范围均在75~400mg·L-1之间,其检出限(3s)在0.65~9.06mg·L-1之间。在已知样品的基础上加入3个浓度水平的标准溶液后,按试验方法进行回收试验,测得其回收率在89.9%~115%之间,测定值的相对标准偏差(n=5)在0.35%~2.3%之间。

2.0000g of the tip paper(cut to small pieces of 5 mm×5 mm)were extracted with 20 mL of H2O by shaking with table for 35min.The extract was taken and filtered through 0.22μm filtering membrane.The filtrate was used for HPLC analysis with evaporation light scattering detection(ELSD).ZORBAX SB C18chromatographic column was used as stationary phase,and mixtures of(A)methanol(containing 0.1 mL of trifluoroacetic acid per liter,pH 4.5)and(B)water in various ratios were used as mobile phase in gradient elution.Volume of sample solution injected was 10μL.Under this condition,7sweeteners were effectively separated.Standard curves of the 7sweeteners were prepared by taking the values of peak areas of the sweeteners as abscissas,and the corresponding mass concentrations as ordinates,and the linearity ranges found were same between 70to400mg·L-1,with their detection limits(3s)in the range from 0.65to 9.06mg·L-1.Test for recovery was made by addition of standards of the sweeteners at concentration levels to known samples as matrixes,giving values of average recovery in the range of 89.9%to 115%.RSDs(n=5)of the determined values were found in the range of0.35%to 2.3%.