色谱

色谱 ›› 2014, Vol. 32 ›› Issue (6): 586-590.DOI: 10.3724/SP.J.1123.2014.03001

• 研究论文 • 上一篇    下一篇

超高效液相色谱-三重四极杆质谱联用方法测定血浆和尿液中的α-龙葵碱、α-卡茄碱和茄啶

张秀尧, 蔡欣欣, 张晓艺   

  1. 温州市疾病预防控制中心, 浙江 温州 325001
  • 收稿日期:2014-03-03 修回日期:2014-03-26 出版日期:2014-06-08 发布日期:2014-05-22
  • 通讯作者: 张秀尧
  • 基金资助:

    温州市医学重点学科、温州市第三轮“311”工程建设项目基金（2008012）.

Determination of α-solanine,α-chaconine and solanidine in plasma and urine by ultra-performance liquid chromatography-triple quadrupole mass spectrometry

ZHANG Xiuyao, CAI Xinxin, ZHANG Xiaoyi   

  1. Wenzhou Center for Disease Control and Prevention, Wenzhou 325001, China
  • Received:2014-03-03 Revised:2014-03-26 Online:2014-06-08 Published:2014-05-22

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摘要：

建立了超高效液相色谱-三重四极杆质谱联用方法，检测血浆和尿液中的α-龙葵碱、α-卡茄碱和茄啶。样品经2%（v/v，下同）甲酸水溶液等量稀释，再经混合型阳离子交换固相萃取柱（MCX SPE）净化，以0.1%甲酸乙腈溶液和含0.05%甲酸的5 mmol/L乙酸铵水溶液作为流动相进行梯度洗脱，在UPLC BEH C18色谱柱上实现分离，正离子电喷雾串联质谱多反应监测（ESI-MS/MS MRM）方式检测，基质匹配外标法定量。一次进样分析时间为5.5 min。血浆和尿液中3种待测物的线性范围均为0.3~100 ng/mL，相关系数为0.997~0.999；样品的检出限为0.1 ng/mL，定量限为0.3 ng/mL；血浆和尿液中的平均加标回收率分别为82%~112%和96%~114%，相对标准偏差为4.0%~16%和2.7%~17% （n=6）。方法简单、准确、灵敏，适用于马铃薯中毒检测。

关键词: α-卡茄碱, α-龙葵碱, 超高效液相色谱-三重四极杆质谱, 串联质谱, 马铃薯, 尿液, 茄啶, 血浆

Abstract:

An ultra-performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-MS/MS) method was developed for the determination of α-solanine,α-chaconine and solanidine in plasma and urine. The sample was acidified with aqueous solution containing 2% (v/v if not specified) formic acid, and then cleaned-up by solid-phase extraction with a mixed-mode cation exchange (MCX) cartridge. The analysis of the glycoalkaloids was carried out on an Acquity UPLC BEH C18 column (50 mm×2.1 mm, 1.7 μm) with gradient elution of acetonitrile (containing 0.1% formic acid) and H2O (containing 0.05% formic acid and 5.0 mmol/L ammonium acetate). The analytes were detected by positive electrospray ionization tandem mass spectrometry in MRM mode, and quantified by external matrix-matched standard calibration. The cycle time of each analysis was 5.5 min. The calibration curves were linear in the range of 0.3-100 ng/mL of the glycoalkaloids in plasma and urine. The correlation coefficients were 0.997-0.999. The limits of detection (S/N=3) and quantitation (S/N=10) were 0.1 ng/mL and 0.3 ng/mL. The average recoveries were 82%-112% and 96%-114% for the glycoalkaloids spiked in plasma and urine, respectively, with relative standard deviations of 4.0%-16% and 2.7%-17% (n=6). The method is simple, accurate and sensitive to detect the glycoalkaloids in plasma and urine for both clinical and forensic purposes.

Key words: α-chaconine, α-solanine, plasma, potato, solanidine, tandem mass spectrometry, ultra-performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-MS/MS), urine

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