高效液相色谱法测定凉皮中的脱氢乙酸

Determination of dehydroacetic acid in Liang Pi by high performance liquid chromatography

中文关键词:  高效液相色谱  凉皮  脱氢乙酸

英文关键词:High performance liquid chromatography  HPLC  Liang Pi  Liangpi  dehydroacetic acid  DHA

中文摘要:

      目的 建立凉皮及其制品中脱氢乙酸含量的高效液相色谱测定方法。方法 样品用水提取,经过0.45 μm微孔过滤膜过滤后进样分析。色谱柱：CNW_? Athena C18-WP色谱柱(250 mm×4.6 mm, 5 μm)；流动相：10 mmol/L乙酸铵水溶液(90%),甲醇(10%)；洗脱方式：等度；检测器波长：230 nm；流速：1.0 mL/min；柱温：室温；进样量：3.0 μL；采用色谱峰保留时间定性,外标法峰面积定量。结果 脱氢乙酸平均回收率98.9%～100%,相对标准偏差0.730%～1.81%,在1μg/mL～50 μg/mL范围内线性良好,相关系数0.9994,定量限10 mg/kg。结论 该方法具有样品预处理简单,分析速度快,灵敏度高的特点。针对厦门市流通领域中的样品实际检测,发现流动商贩所售凉皮制品中脱氢乙酸含量多数超过1.0 g/kg的限量规定。

英文摘要:

      Objective To establish a HPLC method for determination of dehydroacetic acid in Liang Pi. Method use pure water to extract sample and analysis sample after filtering with 0.45 μm microfiltration membrane. Column: CNW C₁₈ column (250 mm × 4.6 mm, 5 μm); mobile phase: 10 mmol/L ammonium acetate solute (90%), methanol (10%); Elution mode: isocratic; detection wavelength: 230 nm; flow rate: 1.0 mL / min; column temperature: room temperature; injection volume: 3.0 μL; external standard method was used to determine the results. Results the analytical results show that the recoveries of dehydroacetic acid in Liang Pi in the range of 98.9%～100%, and the relative standard deviation is 0.730%～1.81%. Linearity of the method in the range 1.0-50.0 μg/mL is good with the correlation coefficients (r₂) of 0.999 4. the limit of quantity (LOQ) of the method is 10 mg/kg. Conclusion The sample preparation of the method is simple, rapid and high sensitivities. The testing result of the actual sample from Xiamen circulation indicated that most of Liangpi product sold by itinerant trader exceed the 1.0 g/kg limited provisions for dehydroacetic acid.