Li Jing, Xu Jicang, Li Xuemei, Zhou Jianguang, Zhu Yan, Miao Mingming
Yunnan Academy of Tobacco Science, Kunming 650106, China.
Se Pu. 2012 Aug;30(8):816-21. doi: 10.3724/sp.j.1123.2012.03029.
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 x 2.1 mm, 1.7 microm) 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 degrees C, and detected by a diode array detector scanned from 200 nm to 500 nm. The regression equations revealed acceptable linearity (correlation coefficients ranged from 0.995 0 to 0.999 9) 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.
建立了一种超高效液相色谱法,用于分离和测定香精香料样品中的14种受限物质。样品用含1%(v/v)氨水的10%(v/v)甲醇水溶液萃取。14种分析物在Waters BEH C18柱(50 mm×2.1 mm,1.7μm)上于12分钟内分离,以乙腈和10 mmol/L醋酸铵水溶液(含0.1%(v/v)乙酸)为流动相,在35℃下以0.2 mL/min的流速进行梯度洗脱,并用二极管阵列检测器在200 nm至500 nm波长范围内进行扫描检测。回归方程表明,14种分析物在0.10 - 50 mg/L范围内具有良好的线性关系(相关系数范围为0.995 0至0.999 9)。检测限为0.32 mg/kg至2.51 mg/kg。14种分析物在实际样品中添加浓度为5、10和20 mg/L时的回收率为93.0% - 121%,相对标准偏差(RSD)为0.51% - 4.50%。该方法具有操作简便、灵敏度高和重现性好等优点,可用于同时测定香精香料样品中的受限物质。