色谱

色谱 ›› 2018, Vol. 36 ›› Issue (1): 12-16.DOI: 10.3724/SP.J.1123.2017.09028

• 研究论文 • 上一篇    下一篇

低温分配固液萃取结合高效液相色谱-质谱法测定食用菌中6-苄基腺嘌呤

侯琨1, 渡边正树2, 王大利3, 韩晶1, 李永路1, 霍虹4   

  1. 1. 日立仪器(大连)有限公司, 辽宁 大连 116033;
    2. 株式会社日立高新技术科学, 日本 茨城 3120033;
    3. 大连市儿童医院, 辽宁 大连 116012;
    4. 中国科学院大连化学物理研究所, 辽宁 大连 116023
  • 收稿日期:2017-09-17 出版日期:2018-01-08 发布日期:2018-01-22
  • 通讯作者: 霍虹,Tel:(0411)84379317,E-mail:huohong21@hotmail.com.

Determination of 6-benzylaminopurine in edible mushrooms by solid liquid extraction with low-temperature partition and high performance liquid chromatography-mass spectrometry

HOU Kun1, WATANABE Masaki2, WANG Dali3, HAN Jing1, LI Yonglu1, HUO Hong4   

  1. 1. Hitachi Instruments(Dalian) Co., Ltd., Dalian 116033, China;
    2. Hitachi High-Tech Science Corporation, Ibaraki 3120033, Japan;
    3. Dalian Children's Hospital, Dalian 116012, China;
    4. Dalian Institute of Chemical Physics, Chinese Academy of Science, Dalian 116023, China
  • Received:2017-09-17 Online:2018-01-08 Published:2018-01-22

PDF

81

摘要：

建立了低温分配固液萃取（SLE-LTP）技术结合高效液相色谱-质谱（HPLC-MS）测定食用菌中6-苄基腺嘌呤（6-BA）的方法。食用菌样品经乙腈提取和低温分配，采用Hitachi LaChrom C18色谱柱（250 mm×4.6 mm，5 μm）分离，以0.02 mol/L乙酸铵（含0.1%（v/v）冰乙酸）-甲醇（6∶4，v/v）溶液为流动相，等度洗脱，在电喷雾正离子模式下检测，外标法定量。结果表明，6-苄基腺嘌呤在0.05~2.0 mg/L范围内线性关系良好，相关系数为1.0000；方法的检出限和定量限分别为0.006 mg/kg和0.02 mg/kg。加标回收率试验显示在0.1 mg/kg和0.5 mg/kg添加水平下6-苄基腺嘌呤的加标回收率为81.3%~93.7%，相对标准偏差为0.7%~2.4%。该法简单、准确、稳定，可用于食用菌中6-苄基腺嘌呤的检测。

关键词: 6-苄基腺嘌呤, 低温分配固液萃取, 高效液相色谱-质谱, 食用菌

Abstract:

A simple method based on solid liquid extraction with low-temperature partition (SLE-LTP) coupled with high performance liquid chromatography-mass spectrometry (HPLC-MS) was developed for the determination of 6-benzylaminopurine (6-BA) in edible mushrooms. The samples were extracted with acetonitrile followed by low-temperature partition at -30℃ for 4 h. The separation was performed on a Hitachi LaChrom C18 column (250 mm×4.6 mm, 5 μm) with 0.02 mol/L ammonium acetate (containing 0.1% (v/v) glacial acetic acid)-methanol (6:4, v/v) as the mobile phases with isocratic elution. The compound was detected in positive electrospray ionization mode, and quantified by external standard method. The results showed that the limit of detection (LOD, S/N>3) for the analyte was 0.006 mg/kg, and the limit of quantification (LOQ, S/N>10) was 0.02 mg/kg. The calibration curve showed good linear in the range of 0.05-2.0 mg/L, and the correlation coefficient (r2) was 1.0000. The spiked recoveries were between 81.3% and 93.7% with the relative standard deviations (RSDs, n=6) of 0.7%-2.4% at the spiked levels of 0.1 mg/kg and 0.5 mg/kg. The developed method is simple, reliable and can be applied for the accurate determination of 6-BA residue in edible mushrooms.

Key words: 6-benzylaminopurine (6-BA), edible mushrooms, high performance liquid chromatography-mass spectrometry (HPLC-MS), solid liquid extraction with low-temperature partition (SLE-LTP)

中图分类号: