杏仁腈在常用溶剂中的稳定性考察及其在健儿清解液中的含量测定

Stability of Mandelonitrile in Commonly Used Solvents and Its Determination in Jian’er Qingjie Mixture

关键词:  杏仁腈  稳定性  健儿清解液  苦杏仁芳香水  高效液相色谱法

Key words:  mandelonitrile  stability  Jian’er Qingjie mixture  almond aromatic water  HPLC

摘要:

目的 采用HPLC考察杏仁腈在常用溶剂中的稳定性并测定健儿清解液中杏仁腈的含量。方法 采用Agilent TC-C₁₈(250 mm×4.6 mm，5 μm)色谱柱，以乙腈−0.1%磷酸溶液(23∶77)为流动相，流速为1.0 mL·min^–1，柱温为30 ℃，检测波长为207 nm。以峰面积的下降率为指标，考察以甲醇、95%乙醇、乙腈、水、pH值2.0~6.0的磷酸溶液及1.0%冰醋酸乙腈为溶剂制备的杏仁腈溶液的稳定性。结果 杏仁腈在甲醇、95%乙醇及水中不稳定，而在乙腈中相对稳定；使用pH值为2.0~3.5的磷酸溶液及1.0%冰醋酸乙腈溶液配制的杏仁腈对照品溶液，可在12 h内保持稳定。杏仁腈质量浓度在1.033~294.987 μg·mL^–1内与峰面积线性关系良好(r=0.999 9)，平均加样回收率为97.4%，RSD为0.6%(n=9)。5家企业生产的16批次样品中杏仁腈的含量为3.854~154.578 μg·mL^–1。结论 所建立的方法简单、准确，可以用于健儿清解液的质量控制；同时应关注溶剂对苦杏仁芳香水及其制剂中杏仁腈稳定性的影响。

Abstract:

OBJECTIVE To establish an HPLC method for investigating the stability of mandelonitrile in commonly used solvents and quantitation determination of mandelonitrile in Jian’er Qingjie mixture. METHODS The assay was performed on an Agilent TC-C₁₈(250 mm×4.6 mm, 5 μm) column with a mobile phase consisting of acetonitrile-0.1% phosphoric acid(23∶27) pumped at a flow rate of 1.0 mL·min^–1. The column temperature was 30 ℃ and the detection wavelength was set at 207 nm. The stability of the mandelonitrile solution prepared with solvents such as methanol, 95% ethanol, acetonitrile, water, phosphoric acid solution with pH 2.0-6.0, and acetonitrile solution containing 1.0% glacial acetic acid was investigated using the peak reduction rate as the indicator. RESULTS Mandelonitrile was labile in methanol, 95% ethanol or water and relatively stable in acetonitrile. The standard solutions of mandelonitrile prepared with phosphoric acid solutions at pH 2.0-3.5 or acetonitrile containing 1.0% glacial acetic acid were stable in 12 h. The linear range of mandelonitrile was 1.033-294.987 μg·mL^–1(r=0.999 9) and the average recovery was 97.4% with RSD of 0.6%(n=9). The content range of mandelonitrile in 16 batches of Jian’er Qingjie mixture produced by 5 manufactures was 3.854-154.578 μg·mL^–1. CONCLUSION The established method is simple and accurate. It can be used for the quality control of Jian’er Qingjie mixture. For almond aromatic water and its preparations, the influence of solvent on stability of mandelonitrile should be noticed.