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  

Determination ofα-solanine,α-chaconine and solanidine in plasma and urine byultra-performance liquid chromatography-triple quadrupole mass spectrometry

作　　者：张秀尧[1] 蔡欣欣[1] 张晓艺[1] 

机构地区：[1]温州市疾病预防控制中心,浙江温州325001

出　　处：《色谱》2014年第6期586-590,共5页Chinese Journal of Chromatography

基　　金：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)

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 C 18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。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 C 18 column（50 mm×2. 1 mm,1. 7 μm）with gradient elution of acetoni-trile（containing 0. 1% formic acid）and H 2 O（ 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 calibra-tion. 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 glycoal-kaloids 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 gly-coalkaloids in plasma and urine for both clinical and forensic purposes.

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

分 类 号：O658[理学—分析化学]