[关键词]
[摘要]
近期不断发现抗炎药物被违法添加到抗风湿保健酒中增加治疗效果,这种现象对消费者健康构成威胁。萘普生是常用非甾体抗炎药物,本研究建立保健食品中违禁添加萘普生的液相检测方法。通过酸性条件氯仿和碱性水溶液两步液-液萃取,从保健酒中提取和净化萘普生。使用Kromasil 100-5C18(250×4.6 mm E74572)色谱柱,以甲醇-0.01M磷酸缓冲液(pH 3.0)(75/25,V/V)流动相,流速为1.0 mL/min进行分离;检测波长为231 nm。通过比对色谱峰保留值和加标实验,结合二极管阵列扫描图谱对可疑样品定性,并根据外标法峰面积定量检测萘普生含量。检品和基质成分基本实现了基线分离,最低检测限为0.5 μg/mL,工作曲线的线性范围: 5~80 μg/mL (R2=0.9993),RSD为1.87% (n=6),加标回收率83.3~92.6%。方法准确、可靠,适用于检测保健品中违法添加的萘普生。
[Key word]
[Abstract]
Recently, undeclared anti-inflammatory drug were frequently exposed being adulterated into antirheumatic health liquors to promote therapeutic effect. This phenomenon poses a serious threat to public health. Naproxen is a common nonsteroidal anti-inflammatory drug. The aim of this study is to develop a liquid chromatographic method coupled with photodiode array detector for identification of illegal adulterated naproxen in healthy food. Two-step liquid-liquid extractions were employed to purify naproxen from samples using chloroform in acidic condition following aqueous solution in alkaline condition, respectively. Chromatographic separation was achieved on a Kromasil 100-5C18 column (250×4.6 mm E74572) with the mobile phase of methanol-10mM phosphate buffer (pH 4.0) (75/25, V/V), at a ?ow rate of 1.0 mL/min. The eluant was detected at 231nm. Retention time combined with standard addition result and PAD-scanning graph were applied to verify naproxen. Quantitation of naproxen was attempted by external standard method. The results showed as follows: the limit of quantitation was 0.5 μg /mL, the linear range was 5~80 μg/mL (R2= 0.9993), RSD was 1.87% (n=6) and the recovery of naproxen from health liquor was ranging from 83.3~92.6%. The method is suitable in determination of naproxen as adulterants in health liquor due to its accuracy and reliability.
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[基金项目]
广东省自然科学基金项目(S2011040001362);韶关市科技计划项目(2013CX/K97)