目的: 建立薄层色谱-近红外光谱(TLC-NIRS)检测方法,用于保健品中违禁化学药物快速定性定量分析。方法: 建立违禁化学药物高效液相色谱(HPLC)含量测定法,作为参考值。采用TLC法,以三氯甲烷-甲醇-甲酸(24∶2∶1)为添加违禁化学药物的展开剂,紫外灯下检视标记,利用NIRS仪分别采集TLC上化学药物斑点的NIRS,采用偏最小二乘法(PLS)结合交叉验证法分别建立化学药物最优定性定量分析模型,并进行模型验证。结果: 所建立的HPLC含量测定方法分离度好,线性范围宽,准确度高。建立的酚酞、呋塞米及盐酸西布曲明TLC-NIRS快速定性定量检测模型经方法学验证,线性范围宽,专属性强,模型稳定性好,预测结果好。建立的酚酞、呋塞米及盐酸西布曲明TLC-NIRS定量分析模型的决定系数(R2)、验证均方差(RMSECV)、预测均方差(RMSEP)分别为0.980、0.085、0.083,0.922、0.106、0.086和0.936、0.091、0.085。应用TLC-NIRS模型对10种减肥保健品进行检测,结果酚酞、呋塞米及盐酸西布曲明含量预测值的平均相对偏差分别为1.75%、1.26%、1.19%。结论: 建立的TLC-NIRS定性定量分析模型通用性强,操作简便,可用于市场上保健品中非法添加上述减肥类化学药物快速检测,为保健品非法添加快速检测研究提供科学思路。
Objective: To establish the detection method of illegally-added anti-obesity drugs by thin layer chromatography (TLC) combined with near-infrared spectroscopy (NIRS), for the rapid qualitative and quantitative analysis of drugs illegally added in health care products. Methods: With the content of chemical drugs in health care products determined by HPLC method as a reference value. Using chloroform-methanol-formic acid (24∶2∶1) as the developing solvent for illegally-added chemical drugs by TLC, the TLC plate was checked and marked under ultraviolet lamp. The NIR spectra of chemical component spots on TLC were collected by NIRS. The rapid qualitative and quantitative model of chemical drugs was established and validated by using the partial least squares regression analysis (PLS) combined with cross validation method. Results: The established HPLC analysis method was accurate with good separation and wide linear range. The established TLC-NIRS analysis models of phenolphthalein, furosemide and sibutramine hydrochloride was specific with wide linear range and good prediction results. The correlation coefficients (R2), the root mean square errors of calibration validation (RMSECV) and the root mean square errors of prediction (RMSEP) were 0.980, 0.085 and 0.083; 0.922, 0.106 and 0.086; 0.936, 0.091 and 0.085, respectively. Ten batches of anti-obesity products were detected by TLC-NIRS model, and the average relative deviations of the contents of phenolphthalein, furosemide and sibutramine hydrochloride of predicted were 1.75%, 1.26% and 1.19%, respectively. Conclusion: The proposed TLC-NIRS analysis models are universal and simple, and can be used for rapid determination of the above chemical components in anti-obesity products, which provide the ideas for rapid determination of illegally-added drugs in health care products.
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