摘要
目的利用高效液相色谱-二极管阵列检测器(HPLC-DAD)技术,建立降糖类保健食品中可能添加的维格列汀、沙格列汀、阿格列汀、利格列汀、恩格列净、达格列净、卡格列净和西格列汀等8种化学药物的检查方法。方法采用Agilent Zorbax C_(18)色谱柱(250 mm×4.6 mm,5μm),以乙腈-0.01 mol·L^(-1)磷酸二氢铵水溶液(含0.04%辛烷磺酸钠,用磷酸调pH至3.3)为流动相,进行梯度或等度洗脱,流速1.0 mL·min^(-1),柱温25℃,检测波长为210、220 nm。结果8种化学成分在对应质量浓度范围内与峰面积呈良好的线性关系(r≥0.9999);低、中、高3个质量浓度的平均回收率均在98.8%~100.7%,RSD在0.44%~0.76%;精密度和稳定性良好,RSD均小于1.0%;检测限为0.022~0.54μg·mL^(-1);定量限为0.070~1.7μg·mL^(-1)。结论该方法简便、准确、易于推广,适用于降糖类保健食品中8种可能非法添加的新型降糖化学药物的检测。
Objective To determine the 8 chemical drugs(vildagliptin,saxagliptin,alogliptin,linagliptin,empagliflozin,dapagliflozin,canagliflozin and sitagliptin)illegally added to antidiabetic dietary supplements by high performance liquid chromatography(HPLC)method with diode array detector(DAD).Methods An Agilent Zorbax C_(18) column(250 mm×4.6 mm,5μm)was used for the separation,with gradient elution or isocratic elution of acetonitrile and aqueous solution of ammonium dihydrogen phosphate(containing 0.04%sodium octane sulfonate and adjusting pH to 3.3 with phosphoric acid)as the mobile phase at the flow rate of 1.0 mL·min^(-1).The column temperature was 25℃,and the detection wavelength was set at 210 and 220 nm.Results Totally 8 chemical constituents showed good linearity between certain mass concentration ranges and the peak area(r≥0.9999).The average spiked recoveries of the low,middle and high levels ranged 98.8%~100.7%(n=9),and the relative standard deviations(RSDs)ranged 0.44%~0.76%.The precisions and stabilities were satisfactory with both RSDs less than 1.0%.Limit of detection and limit of quantity were 0.022~0.54μg·mL^(-1)and 0.070~1.7μg·mL^(-1),respectively.Conclusion The method is simple,accurate and feasible in the detection of 8 new hypoglycemic chemical drugs illegally added in antidiabetic dietary supplements.
作者
徐硕
徐文峰
邝咏梅
金鹏飞
XU Shuo;XU Wen-feng;KUANG Yong-mei;JIN Peng-fei(Department of Pharmaceutical Science,Beijing Hospital,National Center of Gerontology,Institute of Geriatric Medicine,Chinese Academy of Medical Sciences,Beijing Key Laboratory of Assessment of Clinical Drugs Risk and Individual Application(Beijing Hospital),Beijing 100730)
出处
《中南药学》
2023年第7期1911-1916,共6页
Central South Pharmacy