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1．0mL乙腈-水（90＋10，v／v）溶解，过0．22μm滤膜。待测物经WatersUPLCBEHAmide柱分离，选用含2mmol／L乙酸铵的乙腈-水为流动相，10min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1．0～200．0μg／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0．9988～0．9997，土豆样品的最低检测限为0．60μg/kg（α茄碱）和0．21μg／kg（μ卡茄碱），血液或尿液样品分别为0．08μL（α～茄碱）和0．04μg/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。
Objective An ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） method was established for determination of α-solanine and α-chaconinee in food poison- ing samples including potatoes, processed food, vomit, serum, and urine. Methods The samples were extracted with 5 % acetic acid by ultrasonic instrument. For potato sample, the superuatant 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. Results The calibration curves of α-solanine and α-chaconinee in several poisoning samples showed good linearity in the range of 1.0 - 200.0μg/L with correlation coefficient in the range of 0. 998 8 -0.999 7. The detection limit of the method were 0. 60μg/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%, and RSDs of 1.93% 5. 11% were obtained. Conclusion This 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.
出处
《华南预防医学》
2016年第5期435-442,共8页
South China Journal of Preventive Medicine
基金
深圳市科技计划(医药卫生类)资助项目(编号:201302146)
关键词
茄碱
色谱法
高压液相
食物中毒
Solanine
Chromatography, high pressure liquid
Food poisoning
