超高效液相色谱法同时测定香精香料中14种禁限用物质

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

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(50mm×2.1mm,1.7μm),流动相为10mmol/L乙酸铵(含0.1%乙酸)和乙腈,梯度洗脱,流速为0.2mL/min,柱温为35℃,在200～500nm范围内进行扫描检测。结果表明,该方法在12min内可实现14种禁限用物质的分离和检测,在0.10～50mg/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0.32～2.51mg/kg。在5、10、20mg/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。

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.