摘要
目的建立高效液相色谱-荧光检测法(high performance liquidchromatography with fluorescence detector,HPLC-FLD)测定麦卢卡蜂蜜中特征标识物3,5-二甲氧基苯甲酸甲酯-4-双葡萄糖糖苷(leptosperin)的方法。方法以Platisil ODS色谱柱(150 mm×4.6 mm, 5μm)为分析柱,甲醇-水为流动相进行等度洗脱,使用荧光检测器,外标法定量。结果在0.5~100 mg/L范围内目标化合物的线性关系良好,相关系数为0.9999,方法的检出限(limit of detection LOD,S/N≥3)和定量限(limit of quantitation,LOQ,S/N≥10)分别为2mg/kg和8 mg/kg。在10、20、50 mg/kg浓度水平下平均回收率为82.2%~108.9%,相对标准偏差为1.3%~7.5%(n=6)。结论该方法前处理方法简单快速,测定结果准确可靠,可为麦卢卡蜂蜜真伪鉴别提供参考。
Objective To establish a method for the determination of characteristic compound 3,5-dimethoxybenzoate-4-diglucoside (leptosperin) in manuka honey by high performance liquid chromatography with fluorescence detector (HPLC-FLD). Methods The analysis column was Platisil ODS (150 mm×4.6 mm, 5 μm). The samples were dissolved and diluted by methanol-water (30:70, V:V), then analyzed by HPLC-FLD, and external standard method was used for quantification. Results The leptosperin had a good linear relationship in the range of 0.5~100 mg/L (r 2 =0.9999). The limit of detection and limit of quantification of the method were 2 mg/kg and 8 mg/kg, respectively. The recoveries at 3 spiked levels (10, 20, and 50 mg/kg) were 82.2%-108.9%, with the relative standard deviations (RSDs) of 1.3%-7.5% (n=6). Conclusion This method is simple and rapid in pretreatment, accurate and reliable in determination results, which can provide a reference for judging the authenticity of manuka honey.
作者
王雪婷
丁涛
吴斌
刘芸
高玲
唐茂芝
王茂华
郭思言
WANG Xue-Ting;DING Tao;WU Bin;LIU Yun;GAO Ling;TANG Mao-Zhi;WANG Mao-Hua;GUO Si-Yan(Animal, Plant and Food Inspection Center, Lianyungang Entry-Exist Inspection and Quarantine Bureau, Lianyungang 222042, China;Animal, Plant and Food Inspection Center, Jiangsu Entry-Exist Inspection and Quarantine Bureau, Nanjing 210001, China;China Certification & Accreditation Institute, Beijing 100020, China;College of Pharmacy, China Pharmaceutical University, Nanjing 211198, China)
出处
《食品安全质量检测学报》
CAS
2018年第23期6140-6144,共5页
Journal of Food Safety and Quality
基金
国家质检总局科技计划项目(2016IK135)
国家重点研发计划(2017YFF0211000
2018YFF0215605)~~