Objective: To develop a method based on ultra-high-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) for the simultaneous detection of 37 compounds illegally added in Yixintong tablets as an example. Methods: The samples were separated on the UPLC HSS T3 C18(100 mm×2.1 mm, 1.8 μm) chromatographic column by gradient elution using 0.1% formic acid and acetonitrile as the mobile phase. The electrospray ion source was operated in both the positive and negative ion mode using the multi-reaction monitoring(MRM) method, and the results were quantified by the external standard method. Results: The correlation coefficients(R2) of the linear calibration curves were greater than 0.99 in the corresponding mass concentration ranges, and the limits of quantification(LOQs) for the analytes were 3-10 μg·L-1. The average recoveries ranged from 63.4% to 138.3%. Among the 37 compounds to be tested in 78 samples of 46 batches, no other compounds were detected except aspirin. The content of aspirin was 0.847-3.261 μg per tablet, the content was very low and had no significance of illegal addition. Conclusion: The established method is sensitive, rapid, accurate, reliable, and applicable for the detection of the illegal addition of antipyretic and analgesic affect compounds in Yixintong tablets.
ZUO Tian-tian, ZHANG Lin-lin, JIN Hong-yu, WANG Dan-dan, FANG Cui-fen, MA Lin-ke, CHEN Bi-lian, ZAN Ke, MA Shuang-cheng
. Detection of 37 compounds illegally added in Yixintong tablets by ultra- high performance liquid chromatography-tandem mass spectrometry*[J]. Chinese Journal of Pharmaceutical Analysis, 2021
, 41(10)
: 1739
-1747
.
DOI: 10.16155/j.0254-1793.2021.10.11
[1] 史伟, 黄立武, 孙文才, 等. 活血化瘀法治疗糖尿病肾病的概述[J].广西医学, 2002, 24(12): 2002
SHI W, HUANG LW, SUN WC, et al. Summary of promoting blood circulation and removing blood stasis in the treatment of diabetic nephropathy[J].Guangxi Med J, 2002, 24(12): 2002
[2] 中华人民共和国药典2015年版. 一部[S]. 2015: 1402
ChP 2015. Vol Ⅰ[S]. 2015: 1402
[3] 王静文, 曹进, 王钢力, 等. 保健食品中非法添加药物检测技术研究进展[J].药物分析杂志, 2014, 34(1): 1
WANG JW, CAO J, WANG GL, et al. Research progress on determination technologies for illegally added drugs in health food[J].Chin J Pharm Anal, 2014, 34(1): 1
[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] 胡青, 孙健, 冯睿, 等. 超高效液相色谱-三重四极杆质谱法测定食品中34种非法添加减肥类化合物[J].色谱, 2017, 35(6): 594
HU Q, SUN J, FENG R, et al. Determination of 34 illegally adulterated weight loss compounds in foods by ultra high performance liquid chromatography-triple quadrupole mass spectrometry[J].Chin J Chromatogr, 2017, 35(6): 594
[6] 胡青, 孙健, 于泓, 等. 超高效液相色谱-三重四极杆质谱法测定保健食品中28种降糖类非法添加化合物[J].食品安全质量检测学报, 2018, 9(1): 93
HU Q, SUN J, YU H, et al. Determination of 28 anti-diabetic compounds in health foods by ultra performance liquid chromatography-triple quadrupole mass spectrometry[J].J Food Saf Qual, 2018, 9(1): 93
[7] 邢俊波, 曹红, 张炯, 等. 高效液相色谱法同时测定补肾壮阳类中成药及保健食品中非法添加7种化药成分[J].时珍国医国药, 2014, 25(2): 451
XIN JB, CAO H, ZHANG J, et al. Simultaneous determination of 7 illegal components illegally added in traditional Chinese medicine and health food by HPLC[J].Lishizhen Med Mater Med Res, 2014, 25(2): 451
[8] 秦剑红. TLC-SERS联用法检测降糖中成药中添加的格列类药品[J].药学实践杂志, 2014, 32(3): 206
QIN JH. Detection of glinides adulterated in traditional Chinese medicine for diabetes by TLC-SERS[J].J Pharm Pract, 2014, 32(3): 206
[9] 张宏莲, 李莉, 许凤, 等. 薄层色谱法检测降糖中药及保健品非法添加的双胍类成分[J].科技创新导报, 2013, 255(3): 252
ZHANG HL, LI L, XU F, et al. TLC building of biguanide illegally mixed into hypoglycemic proprietary Chinese medicines and health food[J].Sci Technol Innov Her, 2013, 255(3): 252
[10] 汪琪, 苏晶, 覃红萍, 等. TLC法快速筛查降糖类中成药及保健食品中添加的11种化学药品[J].中国药事, 2010, 24(7): 647
WANG Q, SU J, QIN HP, et al. Determination of eleven antidiabetics illegally adulterated into Chinese patent drugs and health foods by TLC[J].Chin Pharm Aff, 2010, 24(7): 647
[11] 吴公平, 雷玉萍, 李荣玮, 等. 采用反相高效液相色谱法测定降糖类保健食品非法添加降糖化学药品检验方法的研究[J].中国现代医学杂志, 2010, 20(9): 1380
WU GP, LEI YP, LI RW, et al. Identification of eleven components of diabetes medicine added illegally to health products by HPLC[J].Chin J Mod Med, 2010, 20(9): 1380
[12] 吴卫涛. 高效液相色谱法同时鉴定保健品中非法添加的6种降糖药成分[J].现代中西医结合杂志, 2009, 18(22): 2703
WU WT. Simultaneous determination of 6 kinds of hypoglycemic ingredients illegally added in health food[J].Mod J Integr Tradit Chin Wes Med, 2009, 18(22): 2703
[13] 曾茂法, 张学斌. 高效液相色谱法同时鉴定保健品中非法添加的四种降糖药成分[J].中国现代应用药学, 2006, 23(6): 506
ZENG MF, ZHANG XB. Identification of four components of diabetes medicine added illegally to health products by HPLC[J].Chin J Mod Appl Pharm, 2006, 23(6): 506
[14] SHANG J, HE X, XI C, et al. Determination of the potential illegal addition of β-blockers to function foods by QuEChERS sample preparation and UPLC-MS/MS analysis[J].Food Addit Contam Part A Chem Anal Control Expo Risk Assess, 2015, 32(7): 1040
[15] 刘波, 袁利鹏, 聂燕华, 等. 氟西汀快速免疫检测用人工抗原的合成与鉴定[J].现代食品科技, 2016, 32(8): 290
LIU B, YUAN LP, NIE YH, et al. Synthesis and identification of artificial antigen for the rapid immunological detection of fluoxetine[J].Mod Food Sci Technol, 2016, 32(8): 290
[16] VAYSSE J, GILARD V, BALAYSSAC S, et al. Identification of a novel sildenafil analogue in an adulterated herbal supplement[J].J Pharm Biomed Anal, 2012, 59: 58
[17] PANG W, YANG H, WU Z, et al. LC–MS-MS in MRM mode for detection and structural identification of synthetic hypoglycemic drugs added illegally to‘natural’ anti-diabetic herbal products[J].Chromatographia, 2009, 70: 1353
[18] ZHOU Z, ZHANG J, ZHANG W, et al. Rapid screening for synthetic antidiabetic drug adulteration in herbal dietary supplements using direct analysis in real time mass spectrometry[J].Analyst, 2011, 136(12): 2613