小儿化毒系列制剂中非法添加松香酸的检测方法研究

Research on Determination of Illegal Additive Abietic Acid in Xiaoerhuadu Series Preparations

目的建立小儿化毒系列制剂中非法添加松香酸的检测方法。方法采用HPLC法(UV检测器)对小儿化毒系列制剂中非法添加松香酸进行检测,液相色谱柱:C18色谱柱,流动相:乙腈-四氢呋喃-0.1%甲酸(45:25:30);流速:1.0 m L·min^(-1);检测波长:241 nm;柱温:30℃。同时采用HPLC-DAD和HPLC-MS法对松香酸检测阳性结果进行进一步的确证。结果松香酸在25.72~321.5 ng的浓度范围内与峰面积呈良好的线性关系,回归方程为Y=0.038 1X+1.698 1,相关系数为0.999 7,检测限为18.4μg·g^(-1)。经检验,确证56批样品有5批检出松香酸。结论此方法简便可行,灵敏度高,可以有效筛查小儿化毒系列制剂中是否掺有松香酸。

Objective To establish a method for detection of illegal additive abietic acid in Xiaoerhuadu series preparations. Methods Illegal additive abietic acid in Xiaoerhuadu series preparations was determined by HPLC-UV method. The HPLC method was carried on C18 column using acetonitrile, tetrahydrofuran and 0.1% formic acid （45：25：30） as the mobile phase to gradient elution, and the flow rate was 1.0 mL ·min-1, the column temperature was 30℃ and the detection wavelength was 241 nm. Then the positive results were confirmed by HPLC-DAD detector and HPLC-MS. Results The linear range of abietic acid was 25.72 -321.5 ng. The regression equation was Y=0.038 1X＋1.698 1 while the correlation coefficient was 0.999 7. The detection limit was 18.4 μg · μg-l. Abietic acid was found in five out of fifty-six batches of samples. Conclusion The method is convenient, sensitive and effective in screening for illegal additive abietic acid in Xiaoerhuadu series preparations.