色谱

色谱 ›› 2012, Vol. 30 ›› Issue (10): 980-985.DOI: 10.3724/SP.J.1123.2012.08026

• 专栏 • 上一篇    下一篇

高效液相色谱-离子阱飞行时间质谱对保健食品中激素类成分的快速筛查和确证

王美玲1, 颜鸿飞1, 傅善良1, 张帆2, 姚劲挺3, 戴华1, 李拥军1,2*   

  1. 1. 湖南出入境检验检疫局技术中心, 湖南 长沙 410004; 2. 食品安全科学技术湖南省重点实验室, 湖南 长沙 410004; 3. 岛津国际贸易(上海)有限公司, 上海 200052
  • 收稿日期:2012-08-17 修回日期:2012-09-07 出版日期:2012-10-28 发布日期:2012-10-17
  • 通讯作者: 李拥军,研究员,主要从事食品中农兽药残留的检测. Tel: (0731)85627820, E-mail: Liyj@hnciq.gov.cn.
  • 基金资助:

    “十二五”科技支撑计划项目(2012BAD33B02).

Rapid screening and confirmation of hormones in health foods by high performance liquid chromatography-ion trap-time of flight tandem mass spectrometry

WANG Meiling1, YAN Hongfei1, FU Shanliang1, ZHANG Fan2, YAO Jinting3, DAI Hua1, LI Yongjun1,2*   

  1. 1. Inspection and Quarantine Technology Center, Hunan Entry-Exit Inspection and Quarantine Bureau, Changsha 410004, China; 2. Hunan Key Laboratory of Food Saftey & Science Technology, Changsha 410004, China; 3. Shimadzu International Trading (Shanghai) Co., Ltd., Shanghai 200052, China
  • Received:2012-08-17 Revised:2012-09-07 Online:2012-10-28 Published:2012-10-17

PDF

518

被引次数

28

摘要： 采用高效液相色谱-离子阱飞行时间串联质谱(HPLC-IT-TOF-MS)对保健食品中雌激素、雄激素、糖皮质激素和二羟基苯甲酸内酯类药物等21种激素成分进行快速筛查、定性识别和准确定量。样品经含1.0%乙酸的乙腈溶液超声提取,提取液经QuEChERS吸附剂净化,以C18色谱柱(150 mm×2.0 mm, 3.0 μm)分离,乙腈和0.1%乙酸水溶液为流动相梯度洗脱,正、负离子模式同时扫描。结果表明,21种化合物在5.0～250 μg/L范围内呈良好的线性相关性,相关系数均大于0.993。胶囊和口服液样品中各化合物的定量限(以信噪比≥10计)分别为2.0～5.0 μg/kg和1.0～2.5 μg/L。在低、中、高3个添加水平下,各化合物的平均回收率为60.2%～116.0%,相对标准偏差(RSD)为7.0%～18.3%。该方法利用精确质量数匹配和自建标准谱库检索,实现快速筛查,并使用多级特征碎片离子进行确证,具有简便、快速、高效、准确等优点,适用于保健食品中多种激素的快速筛查和测定。

关键词: 保健食品, 高效液相色谱-离子阱飞行时间串联质谱, 激素, 筛查

Abstract: A method was developed for the screening, confirmation and quantification of 21 hormones including progesterones, etrogens, glucocorticoids and resorcylic acid lactones in health foods by high performance liquid chromatography-ion trap-time of flight tandem mass spectrometry (HPLC-IT-TOF-MS). The analytes in the sample were extracted with acetonitrile containing 1.0%(v/v) acetic acid and the extract was purified with the mixed QuEChERS sorbents. In the chromatographic analysis, the 21 target compounds were separated on a C18 column with the gradient elution using the mobile phases of acetonitrile and water containing 0.1% acetic acid. The mass analyzer was performed in positive and negative full scan modes in one injection at the same time. The results showed that the linear ranges of the 21 hormones were 5.0~250 μg/L with the correlation coefficients above 0.993 and the limits of quantification (LOQ, S/N≥10) were 2.0~5.0 μg/kg and 1.0~2.5 μg/L for capsule and oral solution, respectively. The method validation was carried out at three spiked levels, and the recoveries were 60.2%~116.0% with the relative standard deviations (RSDs) of 7.0%~18.3%. The screening of analytes was performed by precision mass matching and library searching. The secondary fragment ion spectra were employed to the confirmation. This method is simple, fast, reliable, and can be applied to the simultaneous screening and determination of hormones in health foods.

Key words: health foods, hormones, screening, high performance liquid chromatography-ion trap-time of flight tandem mass spectrometry (HPLC-IT-TOF-MS)