Driedger D R, Sporns P
University of Alberta, Department of Agriculture, Food, and Nutritional Science, Edmonton, Canada.
J AOAC Int. 1999 Jul-Aug;82(4):908-14.
Matrix-assisted laser desorption and ionization (MALDI) mass spectrometry was used to determine concentrations of individual potato glycoalkaloids in tubers. Samples were extracted with methanol-water and deposited on 2,4,6-trihydroxyacetophenone crystals. Positive ions were analyzed with a MALDI time-of-flight mass spectrometer equipped with a 337 nm laser. Analyte ion intensities relative to an internal standard were used to determine chaconine and solanine concentrations. Calibration curves were prepared by standard additions to potato tuber material. The relative standard deviations (RSDs) of triplicate measurements ranged from 1 to 16%, with an average of 9%. The day-to-day RSD for replicate determinations was 11%. Recoveries of analyst-prepared spikes (50 micrograms/g) averaged 104% for chaconine (RSD, 8%) and 98% for solanine (RSD, 4%). The method limit of detection was estimated to be 2 micrograms/g.
采用基质辅助激光解吸电离(MALDI)质谱法测定块茎中各马铃薯糖苷生物碱的浓度。样品用甲醇 - 水提取,并沉积在2,4,6 - 三羟基苯乙酮晶体上。使用配备337 nm激光的MALDI飞行时间质谱仪分析正离子。相对于内标的分析物离子强度用于测定查茄碱和茄碱的浓度。通过向马铃薯块茎材料中添加标准品来制备校准曲线。三次重复测量的相对标准偏差(RSD)范围为1%至16%,平均为9%。重复测定的每日RSD为11%。分析人员制备的加标样品(50微克/克)中,查茄碱的平均回收率为104%(RSD,8%),茄碱的平均回收率为98%(RSD,4%)。该方法的检测限估计为2微克/克。