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目的建立辣椒粉中的碱性橙和碱性玫瑰精的高效液相色谱-串联四极杆质谱测定方法。方法样品经乙腈超声提取后,经ODS-C18和乙二胺-N-丙基硅烷(PSA)的固相分散净化后直接进样分析。使用安捷伦Zobax Eclipse Plus-C18(2.1 mm×100 mm,1.8μm)色谱柱分离,以5 mmol/L乙酸铵-0.1%甲酸-乙腈为流动相,流速为0.25 mL/min。采用电喷雾离子化源,以多反应监测(MRM)方式分析,正离子化进行检测。结果碱性橙和碱性玫瑰精的线性范围为5~1000μg/L,相关系数良好。辣椒粉中碱性橙和碱性玫瑰精的检出限分别为2μg/kg和0.5μg/kg,该方法在三个水平上添加回收率为88.1%~106.4%,相对标准偏差为5.3%~11.7%。结论本方法灵敏度高,操作简单高效,适合于辣椒粉中碱性橙和碱性玫瑰精的定量及确证分析。
OBJECTIVE To establish a method for the determination of basic orange and basic rosehip in paprika by high performance liquid chromatography-tandem quadrupole mass spectrometry. Methods The samples were extracted by acetonitrile and purified by solid-phase dispersion of ODS-C18 and ethylenediamine-N-propylsilane (PSA). Separation was performed using an Agilent Zobax Eclipse Plus-C18 (2.1 mm × 100 mm, 1.8 μm) column with 5 mmol / L ammonium acetate-0.1% formic acid-acetonitrile as the mobile phase at a flow rate of 0.25 mL / min. The electrospray ionization source was used to analyze in multi-reaction monitoring (MRM) mode and positive ionization was performed. Results The linear range of basic orange and basic rose essence was 5 ~ 1000μg / L, the correlation coefficient was good. The detection limits of alkaline orange and basic rose essence in paprika were 2μg / kg and 0.5μg / kg, respectively. The recoveries of three methods were 88.1% -106.4% and the relative standard deviations were 5.3% ~ 11.7%. Conclusion The method has high sensitivity, simple and efficient operation and is suitable for quantitative and confirmatory analysis of basic orange and basic rose essences in paprika.