高压液相色谱法测定柑橘类水果中的 柑橘红 2 号染料

Determination of citrus red 2 in citrus by high perssure liquid chromatography

中文关键词:  柑橘红 2 号  高压液相色谱  柑橘

英文关键词:citrus red 2  high pressure liquid chromatography  citrus

中文摘要:

      目的 建立高压液相液相色谱法(HPLC)测定柑橘类水果中柑橘红 2 号染料的方法。方法 样品用乙腈提取, NH2固相萃取小柱净化后, 用Waters Sunfire C18(250 mm×4.6 mm, 5.0 μm)色谱柱进行分离, 水-乙腈作为流动相, 进行梯度洗脱, 流速为1.0 mL/min. 结果 方法的线性范围为: 0.5~5.0 μg/mL (r=0.99973), 检出限为0.003 mg/kg, 定量限为0.01 mg/kg。在6 个不同种类的柑橘中, 添加柑橘红2 号染料浓度为0.1、0.5、2.0 mg/kg 3 个水平, 回收率在79.48 %~93.20%之间, 相对标准偏差为6. 5% ~ 14.5 %。 利用该方法对市场上随机采集的36 份柑橘样品进行了检测, 其中, 3 份样品有检出。结论 该方法灵敏度高, 准确度好, 适用于对柑橘类样品中柑橘红 2 号染料的检测。

英文摘要:

      Objective To establish a rapid method for the determination of citrus red 2 (CR2) in citrus by high pressure liquid chromatography (HPLC). Methods The samples were extracted with acetonitrile, cleaned-up by NH2 solid phase extraction cartridge. Then, the samples were separated on a Waters Sunfire C18 (250 mm×4.6 mm, 5.0 μm) in gradient elution with the mobile phases of water and acetonitrile. The separated compounds were detected with UV/VIS detector. The linearity of the method (r = 0.99973) was good over the concentration range from 0.5 to 5.0 μg/mL for CR2. The limit of detection (LOD) was 0.003 mg/kg, and the limit of quantification (LOQ) was 0.01 mg/kg. Results The average recoveries of CR2 at 3 levels of 0.1, 0.5 and 2.0 mg/kg were between 79.48 % and 93.20 % with the relative standard deviations (RSDs) between 6.5 % and 14.5 %. A total of 36 citrus samples randomly collected from different markets were detected by the pro-posed method. The results showed that 3 samples contained citrus red 2. Conclusion The sensitivity, accuracy, and precision of this method could meet the requirements of the CR2 analysis.