应用高效液相色谱－二极管阵列检测器筛查中药及保健品中糖皮质激素类非法添加剂  

Detection of glucocorticoids illegally adulterated into traditional chinese medicines and health foods by HPLC-DAD

作　　者：徐巧玲[1] 吴学军[2] 姜文清[2] 邝咏梅[2] 金鹏飞[2] 蔡小兵 

机构地区：[1]解放军第三0五医院,北京100017 [2]北京医院药学部 [3]中央军委联合参谋部警卫局卫生保健处

出　　处：《中国临床保健杂志》2016年第6期569-573,共5页Chinese Journal of Clinical Healthcare

基　　金：中央保健科研课题专项资金(B2009B032)

摘　　要：目的：探讨应用高效液相色谱－二极管阵列检测器（HPLC-DAD）技术建立中药及保健品中非法添加氢化可的松琥珀酸钠、泼尼松龙、氢化可的松、泼尼松、甲泼尼龙、倍他米松、地塞米松、曲安奈德、醋酸泼尼松龙、醋酸氢化可的松、醋酸氟氢可的松、醋酸泼尼松、醋酸可的松、醋酸地塞米松、丁酸氢化可的松、醋酸曲安奈德、醋酸氟轻松和哈西奈德等18种糖皮质激素类添加剂成分的检查方法。方法采用 Alltima C18色谱柱（4．6 mm×250 mm，5μm），流动相为乙腈-10 mmol／L 醋酸铵二元梯度洗脱，流速为0．5 mL／min，检测波长242 nm。对于 HPLC-DAD 检出的疑似阳性样品用液相色谱－质谱法（LC-MS ／MS）进行进一步确认。结果氢化可的松和泼尼松的色谱峰重叠，其他16种糖皮质激素在5～320 mg／L 内线性关系良好，线性相关系数（r）均大于0．9998；灵敏度高，最低检测限均在0．49～0．51 ng 之间，定量限均在1．23～1．27 ng 之间；回收率良好，低、中、高3个浓度的回收率均在97．52％～104．2％之间；精密度良好，相对标准偏差（RSD）均小于0．47％；稳定性良好，12 h 内峰面积和保留时间的相对标准偏差（RSD）均小于0．68％。14种不同剂型的样品通过 HPLC-DAD 检查和 LC-MS ／MS 确认，结果显示：某片剂中检测出醋酸地塞米松，某喷雾剂中检出倍他米松。结论HPLC-DAD技术应用快速、灵敏、易推广，可作为筛查药品及保健品中非法添加18种糖皮质激素的检查方法。Objective To detect 18 glucocorticoids （hydrocortisone sodium succinate,prednisolone,hydrocorti-sone ,prednisone, methylprednisolone, betamethasone, dexamethasone, triamcinolone acetonide, prednisolone acetate, hy-drocortisone, fludrocortisone acetate, prednisone acetate, cortisone acetate, dexamethasone acetate, hydrocortisone buty- rate,triamcinolone acetonide acetate, fluocinonide,halcinonide ） illegally adultered into Traditional Chinese Medicines and health foods by establish an HPLC-DAD method. Methods An Alltima C18column（4. 6 mm×250 mm,5μm）was used for the separations, The mobile phase were consisted of acetonitrile - 10 mmol/L ammonium acetate solution by gradient elution. The flow rate was 0. 5 mL/min. The column temperature was 30 °C. The detection wavelength was 242 nm, Suspicious samples were confirmed by LC-MS/MS. Results The peaks of hydrocortisone and prednisone were over-lapped, the linearity and sensitivity for other 16 glucocorticoids were fine with all correlation coeffcients （r） bigger than 0.9998 and all LODs between0.49 - 0.51 ng,The spiked recoveries of low,middle and high levels ranged from 97.5% to 104.2% ; the precisions were satisfactory with all RSDs 〈0.47% ; the stability within 12h was acceptable with the RS- Ds of peak areas and retention times no more than 0. 68% and 0. 35% , Fourteen Traditional Chinese Medicines and health foods were test by HPLC-DAD and LC-MS/MS,and the result showed：dexamethasone acetate was found in a tab-let sample,while betamethasone was found in a spray sample. Conclusion HPLC-DAD is fast and sensitive method for the detection of 18 glucocorticoids illegally adulterated into Traditional Chinese Medicines and health foods.

关 键 词：气相色谱-质谱法 糖皮质激素类 中草药 营养保健品 

分 类 号：R286.0[医药卫生—中药学] O657.72[医药卫生—中医学]