建立了简便、高效、灵敏的液相色谱-串联质谱分析监测马铃薯中主要糖苷生物碱α-茄碱和α-卡茄碱的方法。样品经酸化甲醇提取后,用无水硫酸钠和无水乙酸镁吸收多余的水分后离心,乙腈和甲酸-甲酸铵缓冲溶液为流动相,梯度洗脱,流速为0.4 mL/min,柱温为40 ℃,进样量为5 μL,提取物经色谱柱分离,在电喷雾正离子模式下,采用四级杆质谱仪进行多反应分析。在实验浓度范围内,α-茄碱和α-卡茄碱标准曲线线性良好,相关系数(R2)均大于0.999;在10、50及100 ng/mL添加浓度水平,所得2种分析物的回收率为98.9%～101.6%,相对标准偏差为0.18%～1.41%,检出限和定量限分别为0.3 mg/kg和1.0 mg/kg。对样品进行了分析,并与文献报道方法的前处理提取效果进行了对比,该方法可达到比已知方法更好的效果。对样品加标后分别用该方法和补充方法对比分析,该方法的加标回收率远高于补充方法的加标回收率,进一步证明了该方法的可行性。结果表明,该法操作简单、重现性好、准确度高,完全满足马铃薯中主要糖苷生物碱α-茄碱和α-卡茄碱的分析监测。
A simple, efficient and sensitive method for the determination of α-solanine and α-chaconine in potato was established. Samples were extracted with acidified methanol and then absorbed with excess water by anhydrous sodium sulfate and magnesium acetate. After centrifugation, the acetonitrile and formic acid ammonium buffer solution were mobile phase, gradient elution, the flow rate was 0.4 mL/min, the column temperature was 40 degrees, the injection volume was 5μL, the extract was separated by chromatographic column, and the multi reaction analysis was carried out by four level mass spectrometer under the electrospray ionization mode. In the experimental concentration range, the standard curves of α-solanine and α-chaconine are well linear, and the correlation coefficient (R2) is greater than 0.999; at the concentration levels of 10, 50 and 100 ng/mL, the recoveries of the two analytes are 98.9%-101.6%, the relative standard deviation is 0.18%-1.41%, the detection limit and quantitative limit are 0.3 mg/kg and 1.0 mg/kg respectively. The sample was analyzed and compared with the pre-treatment extraction results reported in the literature. This method can achieve better results than the known methods. Compared with the supplementary method, the recovery rate of this method is much higher than that of the supplementary method, which further proves the feasibility of this method. The results showed that the method was simple, reproducible and accurate, and could be used for the analysis and monitoring of the major glycoside alkaloids in potato.
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