华南预防医学 ›› 2016, Vol. 42 ›› Issue (5): 435-442.doi: 10.13217/j.scjpm.2016.0435

• 论著 • 上一篇    下一篇

超高效液相色谱-质谱法测定食物中毒样品中α-茄碱和α-卡茄碱

刘红河,康莉,廖仕成,刘桂华   

  1. 深圳市疾病预防控制中心,广东 深圳 518055
  • 收稿日期:2016-02-03 出版日期:2016-11-16 发布日期:2016-12-02
  • 作者简介:刘红河(1970—),男,硕士研究生,主任技师,主要从事食品理化检验研究工作

Determination of αlpha-solanine and αlpha-chaconine in food poisoning samples by ultra performance liquid chromatography-tandem mass spectrometry

LIU Hong-he, KANG Li, LIAO Shi-cheng, LIU Gui-hua   

  1. Shenzhen Center for Disease Control and Prevention, Shenzhen 518055, China
  • Received:2016-02-03 Online:2016-11-16 Published:2016-12-02
  • Contact: 深圳市科技计划(医药卫生类)资助项目(编号:201302146)

摘要: 目的建立一种超高效液相色谱-串联质谱联用法测定包括土豆、加工食品、血清及尿液中龙葵素主要成分α-茄碱和α-卡茄碱的确证方法,为龙葵素中毒提供证据和治疗依据。方法粉碎均匀样品用5%乙酸水溶液进行超声提取,对于土豆样品,提取液用乙腈稀释后上机测定;加工食品、患者呕吐物样品、血液和尿液样品的提取液采用MCX固相萃取柱进行净化,用含5%氨水的乙腈洗脱,收集流出液,将流出液在50 ℃水浴下氮吹浓缩至干。加入1.0 mL乙腈-水(90+10,v/v)溶解,过0.22 μm滤膜。待测物经Waters UPLC BEH Amide柱分离,选用含2 mmol/L乙酸铵的乙腈-水为流动相,10 min内梯度洗脱分离α-茄碱和α-卡茄碱;在优化的质谱条件下,采用ESI源、正离子模式、多反应监测方式,外标法定量。结果在浓度范围1.0~200.0 μg/L内α-茄碱和α-卡茄碱在不同基质样品中均有良好的线性关系,相关系数r在0.998 8~0.999 7,土豆样品的最低检测限为0.60 μg/kg(α-茄碱)和0.21 μg/kg(α-卡茄碱),血液或尿液样品分别为0.08 μg/L(α-茄碱)和0.04 μg/L(α-卡茄碱)。方法回收率在82.6%~105.5%之间,RSD为1.93%~5.11%。结论该方法测定各种中毒样品中α-茄碱和α-卡茄碱的残留量简便、快速、准确,可以用于因龙葵素中毒的应急事件处理,为临床治疗提供依据。

Abstract: ObjectiveAn ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was established for determination of α-solanine and α-chaconinee in food poisoning samples including potatoes, processed food, vomit, serum, and urine. MethodsThe samples were extracted with 5% acetic acid by ultrasonic instrument. For potato sample, the supernatant was diluted with acetonitrile and detected by UPLC-MS/MS. For samples of processed food, vomit, serum, and urine, the supernatants were cleaned-up by solid-phase extraction with a mixed mode cation exchange, and eluted with acetonitrile (containing 5% ammonia water). Then the purified solution was concentrated by nitrogen, dissolved with acetonitrile-water (90+10, v/v) and cleaned by 0.22 μm millipore filter. The sample extract was separated on a Waters UPLC BEH Amide column by gradient elution in 10 minutes with acetronitrile-water (containing 2 mmol/L ammonium acetate) as mobile phase. The filtrate was detected by UPLC-MS/MS, identified by electrospray ionization in positive mode using multiple reaction monitoring, and quantified with external standards. ResultsThe calibration curves of α-solanine and α-chaconinee in several poisoning samples showed good linearity in the range of 1.0-200.0 μg/L with correlation coefficient in the range of 0.998 8-0.999 7. The detection limit of the method were 0.60 μg/kg (α-solanine) and 0.21 μg/kg (α-chaconinee) for potato, 0.08 μg/L (α-solanine) and 0.04 μg/L(α-chaconinee) for serum and urine. The recoveries of three spiking levels ranged from 82.6% to 105.5%, andRSDs of 1.93% -5.11% were obtained. ConclusionThis method is simple, rapid, and accurate for the determination of residues of α-solanine and α-chaconinee in poisoning samples and can be used for emergency detection of solanine poisoning.

中图分类号: 

  • R155.3+2