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HPLC-DAD法快速测定降糖类保健食品中13种化学药物*

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  • 武汉药品医疗器械检验所,武汉 430075
第一作者 Tel:(027)65395516; E-mail:qsky0534@163.com
*Tel:(027)65395516; E-mail:181094873@qq.com

收稿日期: 2020-11-10

  网络出版日期: 2024-06-24

Rapid determination of 13 chemical drugs in antidiabetic health foods by HPLC-DAD*

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  • Wuhan Institute for Drug and Medical Device Control, Wuhan 430075, China

Received date: 2020-11-10

  Online published: 2024-06-24

摘要

目的:建立快速检测降糖类保健食品中13 种化学降糖药的HPLC-DAD法并用于实际检测。方法:采用甲醇超声提取样品中的降糖类化学药物,并应用高效液相色谱-二极管阵列检测器法测定其含量。色谱条件:采用Inert Sustain C18色谱柱(4.6 mm×250 mm,5 μm) 进行分离,以甲醇和10 mmol·L-1乙酸铵为流动相进行梯度洗脱,流速为1.0 mL·min-1,柱温为35 ℃,检测波长为235 nm,对13种降糖类化学药物进行定性、定量测定。结果:13种降糖类化学药物在相应的浓度范围内与其对应峰面积呈良好的线性关系,相关系数均大于0.999 8,3个浓度水平回收率(n=6)为78.6 %~111.2 %,RSD为 0.10%~4.5%。应用本法对11种宣称辅助降血糖保健食品样品进行检测,其中4种样品非法添加了降糖类化学药物,且均为复合添加;4种样品均添加了苯乙双胍、格列本脲,2种样品添加罗格列酮,1种样品添加吡格列酮。结论:该方法操作简单,分析速度快,可作为宣称辅助降血糖类保健食品中非法添加的13种化学药物的有效检测方法,能满足实验室的日常检测需求,具有实际应用意义。

本文引用格式

覃娟, 谢柏艳 . HPLC-DAD法快速测定降糖类保健食品中13种化学药物*[J]. 药物分析杂志, 2021 , 41(11) : 1990 -1999 . DOI: 10.16155/j.0254-1793.2021.11.17

Abstract

Objective: To develop and apply a method for the simultaneous determination of 13 drugs in antidiabe-tic health foods by HPLC-DAD. Methods: The samples were extracted by ultrasonic machine with methanol and the contents were determined by HPLC-DAD. The target analytes were separated on Inert Sustain C18 column (4.6 mm×250 mm, 5 μm) with a mobile phase consisting of 10 mmol·L-1 ammonium acetate and methanol by gradient elution at the flow rate of 1.0 mL·min-1 and the column temperature was 35 ℃. The detection wavelength was set at 235 nm for qualification and quantification analysis of 13 antidiabetic chemical drugs. Results: The calibration curves were linear within the ranges of corresponding concentration. The correlation coefficients were above 0.999 8 for all 13 antidiabetic chemical drugs. The recoveries were in the range of 78.6%-111.2% with RSD of 0.10%-4.5% at three spiked levels. In the 11 batches of samples, the hypoglycemic chemicals were found in 4 batches, and all the 4 batches contained more than one drugs, in which phenformin and glidenclamide were found in four samples, rosiglitazone was found in two samples, pioglitazone was found in one sample. Conclusion: The established method is simple, accurate, rapid and reproducible for qualification and quantification of 13 hypoglycemic chemicals in hypoglycemic health products, which can meet the daily testing requirements of the laboratory and has practical application significance.

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