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.
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