食品科学 ›› 2018, Vol. 39 ›› Issue (22): 312-318.doi: 10.7506/spkx1002-6630-201822047

• 安全检测 • 上一篇    下一篇

血浆和尿液中6 种鹅膏毒肽和鬼笔毒肽的超高效液相色谱-串联质谱法测定

肖绍震1,林锋2,傅武胜2,3,4,5,*,魏道智1,*   

  1. (1.福建农林大学生命科学学院,福建?福州 350002;2.福建中医药大学药学院,福建?福州 350122;3.福建省人兽共患病研究重点实验室,福建省疾病预防控制中心,福建?福州 350001;4.福建医科大学药学院,福建?福州 350108;5.福建农林大学食品科学学院,福建?福州 350002)
  • 出版日期:2018-11-25 发布日期:2018-11-21
  • 基金资助:
    福建省科技计划项目(2018Y0007)

Determination of Amatoxins and Phallotoxins in Plasma and Urine by Ultra Performance Liquid Chromatography-tandem Mass Spectrometry

XIAO Shaozhen1, LIN Feng2, FU Wusheng2,3,4,5,*, WEI Daozhi1,*   

  1. (1. College of Life Sciences, Fujian Agriculture and Forestry University, Fuzhou 350002, China;2. College of Pharmacy, Fujian University of Traditional Chinese Medicine, Fuzhou 350122, China;3. Fujian Provincial Key Laboratory of Zoonosis Research, Fujian Center for Disease Control and Prevention, Fuzhou 350001, China;4. College of Pharmacy, Fujian Medical University, Fuzhou 350108, China; 5. College of Food Science, Fujian Agriculture and Forestry University, Fuzhou 350002, China)
  • Online:2018-11-25 Published:2018-11-21

摘要: 建立同时检测血浆和尿液中鹅膏毒肽和鬼笔毒肽的超高效液相色谱-串联质谱方法。采用模仿人食用有毒野生菌的模式给药实验豚鼠,毒素经过胃肠道首过效应后,利用该方法检测两类毒素在豚鼠血浆和尿液中代谢规律。对实验豚鼠灌胃给药,α-鹅膏毒肽、β-鹅膏毒肽、羧基二羟鬼笔毒肽、二羟鬼笔毒肽的剂量分别为1.0、0.486、0.079、0.120?mg/kg(以体质量计),并对给药后不同时间点采集的血液样品和2?h后的尿液样品进行鹅膏毒肽和鬼笔毒肽含量的检测。结果表明,所建方法血浆和尿液中鹅膏肽类毒素的检出限分别为1.0?μg/L和0.3?μg/L;在质量浓度为2~100?μg/L范围内进行3?个水平的加标实验,回收率均在76.8%~109.0%之间,相对标准偏差为1.30%~12.00%(n=6);血浆中α-鹅膏毒肽和β-鹅膏毒肽均在给药2?h后血药质量浓度达到峰值,分别为14.6、7.24?μg/L,在第24小时处于检出限附近或者未检出;所有时间点的血浆均未检出鬼笔毒肽。在给药后第2小时的尿液中检出全部4?种(α-AMA、β-AMA、PHD和PCD)蘑菇毒素,质量浓度在45.9~1?905?μg/L之间。

关键词: 鹅膏毒肽, 鬼笔毒肽, 超高效液相色谱-串联质谱, 血浆, 尿液

Abstract: An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was successfully developed for the simultaneous determination of amatoxins (AMA) and phallotoxins in plasma and urine. Guinea pigs were orally administered with α-AMA, β-AMA, phallacidin (PCD) and phalloidin (PHD) at single doses of 1.0, 0.486, 0.079 and 0.120 mg/kg·bw respectively. Plasma and urine samples at different time points were collected and analyzed by the developed method to study the metabolism patterns of these toxins in laboratory animals. The results showed that the limits of detection (LODs) were 0.3 and 1.0 μg/L for urine and plasma, respectively. The average recoveries at three spiked levels of 2–100 μg/L varied from 76.8% to 109.0% with relative standard deviations (RSDs) of 1.30%–12.00% (n = 6). α-Amanitin and β-amanitin rapidly reached the maximum levels of 14.6 and 7.24 μg/L in plasma, respectively at 2 h after administration. At 24 h, the amanitins were near the LODs or were undetectable. However, the phallotoxins were below the LODs in plasma at all time points investigated. All four toxins were detected at concentrations of 45.9–1 905 μg/L in urine at 2 h after administration.

Key words: amatoxin, phallotoxin, ultra performance liquid chromatography-tandem mass spectrometry, plasma, urine

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