李晶1,2, 徐济仓1, 李雪梅1, 周建光2, 朱岩3, 缪明明1*超高效液相色谱法同时测定香精香料中14种禁限用物质

建立了超高效液相色谱-二极管阵列检测器(UPLC-PDA)同时测定香精香料中14种禁限用物质的方法。样品经10%(v/v)甲醇水溶液(含1%(v/v)氨水)提取后进行UPLC测定。采用的色谱柱为Waters BEH C18柱(50 mm×2.1 mm, 1.7 μm),流动相为10 mmol/L乙酸铵(含0.1%乙酸)和乙腈,梯度洗脱,流速为0.2 mL/min,柱温为35 ℃,在200～500 nm范围内进行扫描检测。结果表明,该方法在12 min内可实现14种禁限用物质的分离和检测,在0.10～50 mg/L范围内具有较好的线性关系,各待测物的线性相关系数均大于0.995,检出限(以信噪比为3计)为0.32～2.51 mg/kg。在5、10、20 mg/L添加水平下待测物的平均回收率为93.0%～121.0%,相对标准偏差为0.51%～4.50%。该方法操作简易,灵敏度高,线性相关性好,重复性佳,可以满足国内对于香精香料样品中禁限用物质的检测要求。

Simultaneous determination of 14 restricted substances in flavor and fragrant by ultra high performance liquid chromatography

An ultra high performance liquid chromatographic method was established for the separation and determination of 14 restricted substances in flavor and fragrant samples.The sample was extracted by 10%(v/v) methanol aqueous solution containing 1%(v/v) ammonia.The 14 analytes were separated in 12 min on a Waters BEH C18 column(50 mm×2.1 mm,1.7 μm) using acetonitrile and 10 mmol/L ammonium acetate aqueous solution(containing 0.1%(v/v) acetic acid) as mobile phases with gradient elution at a flow rate of 0.2 mL/min and 35 ℃,and detected by a diode array detector scanned from 200 nm to 500 nm.The regression equations revealed acceptable linearity(correlation coefficients ranged from 0.9950 to 0.9999) in the range of 0.10-50 mg/L for the 14 analytes.The limits of detection(LODs) were from 0.32 mg/kg to 2.51 mg/kg.The recoveries of the 14 analytes spiked in real samples at 5,10 and 20 mg/L were 93.0%-121% with the relative standard deviations(RSDs) of 0.51%-4.50%.With the advantages of accessibility,high sensitivity and good reproducibility,this simple method can be used in the simultaneous determination of the restricted substances in flavor and fragrant samples.