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目的建立超快速液相色谱-质谱/质谱联用(UFLC-MS/MS)法测定酚酞片中酚酞的量。方法样品以乙醇提取、微孔滤膜滤过、离心后,通过电喷雾离子化(ESI),采用多反应检测(MRM)方式进行正离子检测,用于定量分析的检测离子为m/z 319.0→225.2。采用Shim-pack XR-ODS色谱柱(75 mm×3.0 mm,2.0μm)分离,以乙腈-水-甲酸(55∶45∶0.1)为流动相,体积流量为0.40 mL/min,在3 min内完成酚酞定量分析。结果线性范围为2.5~1 000.0 ng/mL,最低检测限为2.5 ng/mL;日内RSD小于1.85%,日间RSD小于2.56%。结论本方法灵敏度高,分析速度快,操作简单,可作为酚酞片中酚酞质量控制方法。
OBJECTIVE To establish a method for the determination of phenolphthalein in phenolphthalein tablets by ultra-fast liquid chromatography-mass spectrometry / mass spectrometry (UFLC-MS / MS). Methods The samples were extracted with ethanol, filtered through a microporous filter, centrifuged, and electrospray ionization (ESI) was used to detect the positive ions by MRM. The detection ion for the quantitative analysis was m / z 319.0 → 225.2. Separation was performed on a Shim-pack XR-ODS column (75 mm × 3.0 mm, 2.0 μm) using acetonitrile-water-formic acid (55:45:0.1) as mobile phase at a volumetric flow rate of 0.40 mL / min over 3 min Complete phenolphthalein quantitative analysis. Results The linear range was 2.5-1 000.0 ng / mL with the minimum detectable limit of 2.5 ng / mL. The intra-day RSD was less than 1.85% and the intraday RSD was less than 2.56%. Conclusion The method has high sensitivity, fast analysis speed and simple operation, which can be used as the quality control method of phenolphthalein in phenolphthalein tablets.