1. 重庆医科大学药学院
2. 重庆出入境检验检疫局重庆市进出口食品安全工程技术研究中心
3. 中国检验检疫科学研究院
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周春燕, 唐柏彬, 郗存显, 等. 固相萃取/高效液相色谱法同时测定保健食品中7种磺酰脲类降血糖药物[J]. 分析测试学报, 2013,32(10):1212-1216.
Simultaneous Determination of Seven Sulfonylurea Hypoglycemic Agents in Health Care Products by Solid Phase Extraction/High Performance Liquid Chromatography[J]. 2013,32(10):1212-1216.
建立了同时测定保健食品中7种磺酰脲类降血糖药物(格列吡嗪、甲苯磺丁脲、妥拉磺脲、格列齐特、格列本脲、格列美脲和格列喹酮)的固相萃取/高效液相色谱(SPE/HPLC)分析方法。样品经甲醇超声提取,用C18固相萃取柱净化后进行HPLC分析。采用Agilent Zorbax SB-C18色谱柱(250 mm×4.6 mm,5 μm),以乙腈(A)-0.02%磷酸溶液(B)为流动相,梯度洗脱,流速1.0 mL/min,柱温30 ℃,检测波长228 nm。结果表明,7种目标物在0.2~20 μg/mL范围内线性关系良好,相关系数(r)大于0.999 9,检出限(LOD,S/N≥3)均为0.1 mg/kg,在5种不同基质中的加标回收率为81%~115%,相对标准偏差(RSD)小于9%。
A method was established for the simultaneous determination of seven sulfonylurea hypoglycemic agents(e.g.glipizide,tolbutamide,tolazamide,gliclazide,glibenclamide,glimepiride and glurenor) in health care products by solid phase extraction/high performance liquid chromatography(SPE/HPLC).Various samples were extracted with methanol by ultrasound,the extract was cleaned up and concentrated on an LC-C18 SPE column.The chromatographic separation was performed on an Agilent Zorbax SB-C18 column(250 mm×4.6 mm,5 μm) using acetonitrile(A)-0.02% phosphoric acid solution(B) as mobile phase by gradient elution at a flow rate of 1.0 mL/min,a column temperature of 30 ℃ and an ultraviolet(UV) detection wavelength of 228 nm.The seven sulfonylurea hypoglycemic agents showed good linear relationships in the range of 0.2-20 μg/mL with correlation coefficients larger than 0.999 9.The limits of detection(S/N≥3) were 0.1 mg/kg for seven target compounds.The spiked recoveries of seven target compounds in five different health care products ranged from 81% to 115% with relative standard deviations less than 9%.
固相萃取高效液相色谱法保健食品磺酰脲类降血糖药物
solid phase extraction(SPE)high performance liquid chromatography(HPLC)health care productssulfonylurea hypoglycemic agents
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