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建立刺玫果总黄酮中大孔树脂残留物的测定方法。采用顶空气相色谱法测定刺玫果总黄酮中大孔树脂残留物的质量浓度,色谱柱为Rtx-wax石英毛细管柱(30 m×0.32 mm,0.25μm);柱温为程序升温(起始温度为70℃,保持21 min,以30℃·min~(-1)升温至200℃,保持6 min);进样口温度220℃;检测器温度260℃;用二甲亚砜作溶剂,以氮气为载气,氢气为燃气,空气为助燃气。试验结果表明,正己烷、苯、甲苯、对二甲苯、苯乙烯和对二乙基苯6种大孔树脂残留物分离度良好,其峰面积与质量浓度在各自的浓度范围内呈良好的线性关系,各有机溶剂的最低检测限分别为苯0.19 ng/m L、甲苯0.36 ng/m L、对二甲苯0.37 ng/m L、苯乙烯0.33 ng/m L、对二乙基苯0.40 ng/m L以及正己烷0.27 ng/m L,精密度RSD均小于3%,3个浓度的加标回收率平均在98.19%~101.49%之间。结果说明试验建立的顶空气相色谱法精密度高、准确可靠、重现性良好,适用于刺玫果总黄酮中大孔树脂中残留物的含量测定。
Establishment of a method for determination of macroporous resin residues in total flavonoids from Prickly Pear. The mass concentration of macroporous resin residues in total flavonoids of Prunella vulgaris L. was determined by headspace gas chromatography. The column was Rtx-wax quartz capillary column (30 m × 0.32 mm, 0.25 μm) The temperature was 70 ℃ and kept for 21 min, the temperature was raised to 200 ℃ at 30 ℃ · min -1 for 6 min; the inlet temperature was 220 ℃; the detector temperature was 260 ℃; with dimethyl sulfoxide as solvent, Nitrogen as a carrier gas, hydrogen gas, air to help gas. The experimental results showed that the separation of 6 kinds of macroporous resin residues of n-hexane, benzene, toluene, p-xylene, styrene and p-diethylbenzene was good, and the peak area and mass concentration showed good linearity The detection limit of each organic solvent were 0.19 ng / m L of benzene, 0.36 ng / m L of toluene, 0.37 ng / m L of p-xylene, 0.33 ng / m L of styrene and 0.40 ng / m L and n-hexane 0.27 ng / m L, RSDs of precision were all less than 3%. The spiked recoveries of three concentrations were between 98.19% and 101.49% on average. The results showed that the headspace gas chromatography established by the experiment had high precision, accuracy and reliability and good reproducibility. It was suitable for the determination of the residues in the macroporous resin from the total flavonoids of Prickly heat.