超高效液相色谱法同时测定植物提取物中的6种防腐剂.docVIP

超高效液相色谱法测定植物提取物中的6种防腐剂 李晶1,2，徐济仓1，魏玉玲1，杨叶昆1，周建光2，李雪梅1* （1. 云南烟草科学研究院，昆明 650106； 2. 工业控制技术国家重点实验室，浙江大学智能系统与控制研究所，杭州 310058） 摘要：提出了超高效液相色谱－二极管阵列检测器（UPLC－PDA）同时测定植物提取物中6种防腐剂的方法。测定试样利用50%（v/v）甲醇水溶液进行超声提取15 min后，离心分离取上层清液过Waters BEH C18 (1.7 μm, 2.1 mm×50 mm)色谱柱，采用5 mmol/L 乙酸铵（含0.1% 乙酸）和色谱级乙腈(ACN)为流动相梯度淋洗分离，二极管阵列检测器在200～500 nm范围内进行扫描检测，外标法定量。6种防腐剂的线性范围为0.5~50 mg/L, 线性相关系数在0.9987-0.9997之间，方法的检出限（3S/N）为0.2~2.2 mg/kg；通过添加低中高三组标准溶液，回收率在97.8%~114.1%之间，相对标准偏差(RSD, n=5)在1.0%~4.7%之间。 关键词：超高效液相色谱（UPLC）；植物提取物；防腐剂；分离；检测 Simultaneous Determination of 6 Preservatives in Plant Extracts by Ultra High Performance Liquid Chromatography LI Jing1,2, XU Ji-cang1, WEI Yu-ling1, YANG Ye-kun1, ZHOU Jian-guang2, LI Xue-mei1* (1. Yunnan Academy of Tobacco Science , Kunming, 650106, China; 2. State Key Laboratory of Industrial Control Technology, Institute of Cyber-Systems and Control, Zhejiang University, Hangzhou, 310058, China) Abstract: An ultra high performance liquid chromatography method coupled with Photo Diode Array Detector (PDA) as detector was established for the separation and determination of 6 preservatives in plant extracts. The samples were extracted by 50% (v/v) methanol-water solution for 15 min. After centrifugation, the clear supernatant was taken for separation on a Waters BEH C18 column (1.7 μm, 2.1 mm×50 mm) in gradient elution mode using HPLC acetonitrile and 5 mmol/L ammonium acetate aqueous solution (with 0.1% (V/V)) acetic acid) as mobile phases, detected by a diode array detector scanned from 200 nm to 500 nm and quantified by external standard method. Regression equations revealed acceptable linearity (correlation coefficients ranged from 0.9987 to 0.9997) across the working-standard range (0.5-200 mg/L) for the 6 preservatives. The limits of detection (LODs) were further evaluated (from 0.2~2.2 mg/L). The spiked recoveries of real samples (5 mg/L,10 mg/L, 20 mg/L) were in the range of 97.8%~114.1% with the relative standard deviations （RSD）of 1.0%~4.7%. Keywords: U