安全监测

TLC-NIRS联用技术快速检测保健品中添加减肥类化学药物研究*

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  • 1.陕西省安康市食品药品检验检测中心,安康 725000;
    2.北京中医药大学 中药学院,北京 100029
第一作者 Tel:18791071858;E-mail:1570914816@qq.com
** Tel:(0915)3210257;E-mail:715401074@qq.com

收稿日期: 2022-09-28

  网络出版日期: 2024-06-25

基金资助

* 陕西省社会发展科技攻关项目(2015SF286));安康市社会发展科技攻关项目(AK2021-SF-01)

Determination of anti-obesity drugs illegally added in health care products by TLC-NIRS*

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  • 1. Ankang Inspection and Detection Center of Food and Drug Control, Ankang 725000, China;
    2. Department of Chinese Medicine, Beijing University of Chinese Medicine, Beijing 100029, China

Received date: 2022-09-28

  Online published: 2024-06-25

摘要

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。

本文引用格式

张立军, 张新玥, 张转平, 李小安, 徐桂新, 谭华森, 吴春燕, 吴有朵 . TLC-NIRS联用技术快速检测保健品中添加减肥类化学药物研究*[J]. 药物分析杂志, 2022 , 42(11) : 1961 -1971 . DOI: 10.16155/j.0254-1793.2022.11.13

Abstract

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.

参考文献

[1] CONROY DM, GAN C, ERRMANN A, et al. Fortifying wellbeing: how Chinese consumers and doctors navigate the role of functional foods[J].Appetite, 2021,10(12): 105296
[2] 陈洪忠,巩建华. 创新药品监督抽验理念打击中药制剂中非法添加化学物质的违法行为[J].齐鲁药事,2009,28(6):324
CHEN HZ, GONG JH. Innovating the concept of drug supervision and sampling inspection to crack down on illegal activities of illegally adding chemical substances in traditional Chinese medicine preparations[J].Qilu Pharm Aff, 2009, 28(6): 324
[3] 朱健,裘一婧,沈国芳. UPLC-MS/MS法快速检测减肥类保健品中13种非法添加化学成分[J].中草药,2014,45(4):509
ZHU J, QIU YJ, SHEN GF. Rapid determination of 13 compenents illegally add in slimming functional products by UPLC-MS/MS method[J].Chin Tradit Herb Drugs, 2014, 45(4): 505
[4] 徐硕,金鹏飞,徐巧玲,等. 中药及保健品中非法添加化学药物的研究进展[J].中国新药杂志,2015,24(16):1843
XU S, JIN PF, XU QL, et al. Advances in the chemical substances illegally adulterated in traditional Chinese medicines and health foods[J].Chin J New Drugs, 2015, 24(16): 1843
[5] MAGDALENE HY, TANG SAMMY PL, CHEN SW, et al. Case series on a diversity of illicit weight-reducing agents: from the well known to the unexpected[J].British J Clin Pharm, 2011, 71(2): 250
[6] KOJIM A, SATO Y, CHIBA T, et al. Notable adverse events associated with concomitant use of health foods and drugs derived from the analysis of HFNet data on the safety and effectiveness ofhealth foods[J].J Food Hyg Soc Jpn, 2018, 59(2): 80
[7] 许凤,李莉,张宏莲,等. 薄层色谱扫描法对减肥保健食品中酚酞的定性定量分析[J].药物分析杂志,2014,34(9):1634
XU F, LI L, ZHANG HL, et al. Identification and determination of phenolphthalein added into the anti-obesity product and healthcare food by TLCS[J].Chin J Pharm Anal, 2014, 34(9): 1634
[8] 贾昌平,钱叶飞,赵琪,等. 减肥类保健食品中25种非法添加化学物质的UPLC-DAD快速筛查[J].中成药,2018,40(12):2803
JIA CP, QIAN YF, ZHAO Q, et al. Rapid screening of 25 illegally added chemicals in weight-loss health foods by UPLC-DAD[J].Chin Tradit Pat Med, 2018, 40(12): 2803
[9] 詹淑玉,朱琦峰,徐宏祥,等. UPLC-MS/MS法快速测定减肥类中成药及保健食品中非法添加15种化学药的研究[J].中草药,2016,47(17):3023
ZHAN SY, ZHU QF, XU HX, et al. Rapid determination of 15 chemical drugs illegally added into slimming Chinese patent medicines and health foods by UPLC-MS/MS[J].Chin Tradit Herb Drugs, 2016, 47(17): 3023
[10] 朱志鑫,吴惠勤,黄晓兰,等. 气相色谱-质谱法检测减肥食品中芬氟拉明和西布曲明[J].现代食品科技,2012,28(10):1419
ZHU ZX, WU HQ, HUANG XL, et al. Determination of fenfluramine and sibutramine in diet food by GC-MS[J].Mod Food Sci Tech, 2012, 28(10): 1419
[11] 李想,谭丽丽,刘吉成,等. TLC原位拉曼光谱法快速检测减肥类保健食品中非法添加的四种成分[J].光谱学与光谱分析,2018,38(3):830
LI X, TAN LL, LIU JC, et al. Rapid detection of four chemical components added illegally in slimming health food with TLC situ Raman spectroscopy[J].Spectros Spect Anal, 2018, 38(3): 830
[12] 王巍,卢红,周洪,等. 中成药及保健食品中非法添加化学物质快速检测试剂盒的研究进展[J].食品安全导刊,2021,7(7):74
WANG W, LU H, ZHOU H, et al. Research progress of rapid detection kit for illegally added chemicals in Chinese patent medicine and health food[J].China Food Saf Mag, 2021, 7(7): 74
[13] 吕武清. 中成药中的药材薄层色谱鉴别[M].北京:人民卫生出版社,1997:56
LÜ WQ. TLC Identification of Chinese Patent Medicines[M].Beijing:People’s Medical Press, 1997: 56
[14] 严衍禄,陈斌,朱大洲. 近红外光谱分析的原理、技术与应用[M].北京:中国轻工业出版社,2013:102
YAN YL, CHEN B, ZHU DZ. The Principle, Technology and Application of Near-infrared Spectroscopy[M].Beijing:China Light Industry Press, 2013: 102
[15] 白钢,丁国钰,侯媛媛,等. 引进近红外技术用于中药材品质的快速评价[J].中国中药杂志,2016,41(19):3501
BAI G, DING GY, HOU YY, et al. Rapid identification and evaluation of Chinese materia medica quality by near infrared spectroscopy[J].China J Chin Mat Med, 2016, 41(19): 3501
[16] 张立军,贾建忠,张新玥,等. TLC-NIRS联用技术快速检测保健品中非法添加性保健类化学药物研究[J].天然产物研究与开发,2021,33(9):1572
ZHANG LJ, JIA JZ, ZHANG XY, et al. Determination of sex-enhancing drugs illegally added in health care products by TLC-NIRS combined technology[J].Nat Prod Res Dev, 2021, 33(9): 1572
[17] VESELÁ AK, BARROS AS, SYNYTSYA A, et al. Infrared spectroscopy and outer product analysis for quantification of fat, nitrogen, and moisture of cocoa powder[J].Anal Chim Acta, 2007, 601(1): 77
[18] AGUSSABTI A, RAHMADDIANSYAH A, SATRIYO P, et al. Data analysis on near infrared spectroscopy as a part of technology adoption for cocoa farmer in Aceh Province, Indonesia[J].Data Brief, 2020, 12(29): 105251
[19] 李铮,佟旭光. 西布曲明的不良反应研究进展[J].首都医药,2011,18(14):42
LI Z, TONG XG. Research progress on adverse reactions of sibutramine[J].Cap Med, 2011, 18(14): 42
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