高效液相色谱法测定消肿止痛类中成药中16种非法添加糖皮质激素及消炎镇痛类化学成分

HPLC determination of 16 glucocorticoids and anti-inflammatory analgesics illegally added in Chinese traditional patent medicines

目的建立消肿止痛类中成药中16种非法添加糖皮质激素类及消炎镇痛类化学成分的高效液相色谱检测方法。方法供试品经甲醇超声提取,采用Agela C18色谱柱,经乙腈-水和乙腈-0.02mol·L^-1乙酸铵(含0.5%冰醋酸溶液)两个流动相体系分别梯度洗脱,流速1.0 mL·min^-1,柱温35℃,检测波长分别为240、210 nm。结果 16种化学成分(贝诺酯、曲安西龙、氢化可的松、地塞米松、曲安奈德、醋酸泼尼松龙、醋酸氢化可的松、醋酸泼尼松、醋酸地塞米松、醋酸曲安奈德、醋酸氟轻松、氨基比林、阿司匹林、双氯芬酸钠、罗通定、布洛芬)质量浓度在3.06~359μg·mL^-1与峰面积线性关系良好(r> 0.999);平均加样回收率均在87.7%~113.0%。11批供试品中2批检出醋酸泼尼松,阳性率为18%。结论该方法操作简便、结果准确,可用于消肿止痛类中成药中16种非法添加糖皮质激素类及消炎镇痛类化学成分的定性定量测定。

Objective To establish an HPLC method to detect 16 glucocorticoids and anti-inflammatory analgesics illegally added in Chinese traditional patent medicines. Methods After ultrasonic extraction with methanol, the sample was separated on Agela C18 column with gradient elution. The two mobile phases consisted of acetonitrilewater and acetonitrile 0.02 mol·L^-1 ammonium acetate(containing 0.5% formic acid) at 1.0 mL·min^-1. The column temperature was 35 ℃. The detection wavelength was 240 and 210 nm, respectively. Results Totally 16 drugs(benorilate, triamcinolone, hydrocortisone, dexamethasone, triamcinolone acetonide, prednisolone acetate, hydrocortisone acetate, prednisone acetate, dexamethasone acetate, triamcinolone acetonide acetate, fluocinolone acetonide, aminobilin, aspirin, sodium diclofenac, rotundine, and ibuprofen) showed good linear relationship at 3.06-359 μg·m L^-1. The correlation coefficients(r) were greater than 0.999, and the average recoveries were all at 87.7%^-113.0%. Prednisone acetate was detected in 2 of the 11 samples batches. The positive rate was 18%. Conclusion This method is easy to operate, accurate, which can be used for the qualitative and quantitative determination of 16 glucocorticoids and anti-inflammatory analgesics illegally added in Chinese traditional patent medicines.