目的: 建立防风饮片中掺混水防风的检测方法,并将其作为补充检验方法对市场中防风饮片掺伪情况进行研判。方法: 首先采用薄层色谱法(TLC),对水防风区别于防风的特征性成分[3’(S),4’(R)-双当归酰氧基-3’,4’-二氢花椒内酯]进行初筛,如果供试品溶液色谱中出现水防风特征斑点,则采用高效液相液相色谱法(HPLC)对其进行定量,色谱条件:Agilent Extent C18色谱柱(250 mm×4.6 mm,5 μm),乙腈-水(60∶40)为流动相,等度洗脱,流速为1.0 mL·min-1,检测波长为324 nm。如果量值超出拟定限度,则判定防风饮片中掺有水防风。如有必要采用高效液相-质谱联用法(HPLC-MS)进行确证。结果: TLC、HPLC方法专属性、重复性、耐用性均较好,对2019年国家药品抽检的236批次防风饮片进行了检测,其中17批次检出水防风的特征成分[3’(S),4’(R)-双当归酰氧基-3’,4’-二氢花椒内酯],且超过拟定限量,占比为7.2%,存在掺伪情况。结论: 建立的方法可快速进行防风中掺混水防风的定性定量检测,有效地控制防风及其饮片的质量。
Objective: To establish a method for the Libonotis radix mixed in Saposhnikoviae radix pieces and to test the adulteration of Saposhnikoviaeradix in the market as a supplementary inspection method. Methods: Firstly, TLC was used to analyze Saposhnikoviae radix pieces. If the characteristic spots of the characteristic components [3’(S), 4’(R)-didangryloxy-3’, 4’-dihydrozanthoxylide] of Libonotis radix was found, the quantitative analysis was carried out by HPLC. The HPLC assay was performed on a Agilent Extent C18 column (250 mm×4.6 mm, 5 μm) with acetonitrile-water(60∶40)as mobil phase by isocratic elution at a flow of 1.0 mL·min-1. The detection wavelenghth was set at 324 nm.If the value exceeds the limitation, then the Libonotis radix mixed in Saposhnikoviae radix pieces were determine. If necessary the HPLC-MS method can be used to check the 3’(S), 4’(R)-didangryloxy-3’, 4’-dihydrozanthoxylide. Results: The result showed that the characteristic components of Libonotis radix (3’(S), 4’(R)-didangryloxy-3’, 4’-dihydrozanthoxylide) could be detected and exceeds the prescribed limit in 17 of totally 236 batches of random-checked Saposhnikoviae radix, accounting for 7.2%, which was adulterated. Conclusion: TLC and HPLC methods have good specificity, repeatability, and durability and can detect the Saposhnikoviae radix adulteration quickly and effectively, and provides guarantee for the quality of Saposhnikoviae radix and its decoction pieces.
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