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超高效液相色谱法同时测定香精香料中14种限用物质

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

作者信息

Li Jing, Xu Jicang, Li Xuemei, Zhou Jianguang, Zhu Yan, Miao Mingming

机构信息

Yunnan Academy of Tobacco Science, Kunming 650106, China.

出版信息

Se Pu. 2012 Aug;30(8):816-21. doi: 10.3724/sp.j.1123.2012.03029.

Abstract

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.

摘要

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。

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