固相萃取-高效液相色谱测定饲料中新橙皮苷二氢查耳酮和柚皮苷二氢查耳酮

建立了固相萃取-高效液相色谱检测饲料中新橙皮苷二氢查耳酮(NHDC)和柚皮苷二氢查耳酮(Naringin DC)的方法。采用纯甲醇溶液进行超声辅助萃取样品,经HLB固相萃取柱净化后在XB-C18 (150 mm×4.6 mm, 5 μm)色谱柱上分离,用甲醇/水作为流动相进行梯度洗脱,光电二极管阵列检测器进行检测。结果表明,新橙皮苷二氢查耳酮和柚皮苷二氢查耳酮在0.2~49.0 mg/L 范围内具有良好的线性关系,相关系数均>0.999,定量限分别为0.02和0.01 mg/kg 。日内和日间精密度分别为0.7%~4.1%和0.9%~6.0%。方法的加标回收率为86.2%~105.0%,相对标准偏差(RSDs)为1.0%~6.3%( n =3)。该方法能有效降低饲料基体成分的干扰,灵敏度高,重现性好,适用于饲料中新橙皮苷二氢查耳酮和柚皮苷二氢查耳酮的定量检测。

Determination of neohesperidin dihydrochalcone and naringin dihydrochalcone in feeds by solid phase extraction-high performance liquid chromatography

A new method was established for the determination of neohesperidin dihydrochalcone (NHDC) and naringin dihydrochalcone (Naringin DC) in feeds by solid phase extraction-high performance liquid chromatography (SPE-HPLC). The samples were extracted by methanol and were purified on an HLB solid-phase extraction column. Chromatographic separation was achieved on an XB-C₁₈ column (150 mm×4.6 mm, 5 μm) by linear gradient elution using methanol/water as the mobile phase. The analytes were detected by the diode array detector (DAD). The results revealed a good linear correlation (r>0.999) between the peak areas and mass concentrations of dihydrochalcone sweeteners in the range of 0.2-49.0 mg/L. The limits of quantification (LOQs) of NHDC and Naringin DC were 0.02 and 0.01 mg/kg, respectively. Intra- and inter-day reproducibilities were 0.7%-4.1% and 0.9%-6.0%, respectively. The spiked recoveries for the samples and relative standard deviations (RSDs) were 86.2%-105.0% and 1.0%-6.3% (n=3), respectively. It is both sensitive and repeatable for the quantitative determination of neohesperidin dihydrochalcone and naringin dihydrochalcone in feeds, and thus, can be used to effectively reduce interference in feeds.