Rapid determination of 4 anti-diabetic medicines in health foods by high performance liquid chromatography-tandem mass spectrometry
Objective:A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was established for rapid determination of empagliflozin, linagliptin, saxagliptin and alogliptin in health foods.Methods:Target compounds in samples were ultrasonically extracted by methanol, separated by reverse liquid chromatography and detected by electrospray ionization (ESI) using multiple reaction monitoring (MRM) mode. The quantitation was carried out by external standard method of matrix calibration curve.Results:Good linear relationship displayed in the concentration range of 2~100 μg/L for saxagliptin and alogliptin, with the limits of quantitation (LOQs) of saxagliptin and alogliptin of 0.10 mg/kg. At three spiked concentration levels of 0.1, 0.2 and 1.0 mg/kg, the recoveries were 79.2%~113.0%, with relative standard deviations (RSDs) of 0.9%~8.4%. The linear ranges of empagliflozin and linagliptin were 20~500 μg/L with LOQs of empagliflozin and linagliptin were 1.00 mg/kg. The recoveries were 77.5%~111.1% with relative standard deviations(RSDs) of 2.5%~9.4% at three spiked concentration levels of 1.0, 2.0 and 10.0 mg/kg.Conclusion:The method is simple, rapid, accurate and suitable for identification and determination of 4 anti-diabetic medicines in health foods.
Hai-tao; Yu-meng, ZHANG; Yan-hua, YONG; Peng, LI; Li-na, WANG; and Chun-min, SU
"Rapid determination of 4 anti-diabetic medicines in health foods by high performance liquid chromatography-tandem mass spectrometry,"
Food and Machinery: Vol. 38:
2, Article 8.
Available at: https://www.ifoodmm.cn/journal/vol38/iss2/8
 曹梅荣,李强,张冬生,等.超高效液相色谱—串联质谱法快速检测降糖类保健食品中的10种非法添加物[J].分析试验室,2015,34(8):896-901.CAO Mei-rong,LI Qiang,ZHANG Dong-sheng,et al.Fast determination of 10 illegally added components in anti-diabetic health foods by ultra-high performance liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Analysis Laboratory,2015,34(8):896-901.
 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):93-102.HU Qing,SUN Jian,YU Hong,et al.Determination of 28 anti-diabetic compounds in health foods by ultra performance liquid chromatography-triple quadrupole mass spectrometry[J].Journal of Food Safety and Quality,2018,9(1):93-102.
 ZHOU Zhi-gui,ZHANG Jia-ling,ZHANG Wei,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):2 613-2 618.
 朱峰,阮丽萍,马永建,等.超高效液相色谱—串联质谱联用法同时检测降糖类和减肥类保健品中20种非法添加的化学降糖药物[J].色谱,2014,32(1):13-20.ZHU Feng,RUAN Li-ping,MA Yong-jian,et al.Simultaneous determination of 20 illegally added anti-diabetic chemical components in hypoglycemic and weight-reducing health foods by ultra-high performance liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Chromatography,2014,32(1):13-20.
 GUO B,WANG M,LIU Y,et al.Wide-scope screening of illegal adulterants in dietary and herbal supplements via rapid polarity-switching and multistage accurate mass confirmation using an LC-IT/TOF hybrid instrument[J].Journal of Agricultural and Food Chemistry,2015,63(31):6 954-6 967.
 林芳,李涛,王一欣,等.超高效液相色谱法同时测定降糖类保健食品中非法添加的13种化学药物[J].食品科学,2016,37(18):178-184.LIN Fang,LI Tao,WANG Yi-xin,et al.Simultaneous determination of 13 illegally added chemical drugs in hypoglycemic health foods by ultra performance liquid chromatography[J].Food Science,2016,37(18):178-184.
 励炯,曹青文,王姣斐,等.基于实心核颗粒色谱技术结合HPLC法快速测定保健食品中非法添加13种降糖化学成分[J].中草药,2017,48(13):2 666-2 673.LI Jiong,CAO Qing-wen,WANG Jiao-fei,et al.Detection of 13 anti-diabetic drugs illegally added in health food by HPLC with solid nuclear particle chromatographic column[J].Chinese Traditional and Herbal Drugs,2017,48(13):2 666-2 673.
 郭莉君,董梅,王嘉林,等.基于风险分析建立保健食品中非法添加不同类型化学降糖药的分析方法[J].中国药师,2018,21(11):2 070-2 073.GUO Li-jun,DONG Mei,WANG Jia-ling,et al.Analytical method establishment for the determination of different types of illegally added anti-diabetic chemical components in health foods based on risk analysis[J].China Pharmacist,2018,21(11):2 070-2 073.
 汪祺,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):647-649.WANG Qi,SU Jing,QIN Hong-ping,et al.Determination of eleven antidiabetics illegally adulterated into chinese patent drugs and health foods by TLC[J].Chinese Pharmaceutical Affairs,2010,24(7):647-649.
 田国贺,王梓巍,单元春.NIR快速筛选降糖类中药及保健食品中非法添加盐酸二甲双胍的方法研究[J].中国现代中药,2014,16(1):17-20.TIAN Guo-he,WANG Zi-wei,SHAN Yuan-chun.Establishing NIR method rapidly checking the illegally adding metformin hydrochloride in traditional chinese medicine and health products[J].Modern Chinese Medicine,2014,16(1):17-20.
 刘波,吴婷婷,侯玉兰,等.解吸附电晕束电离质谱法快速检测功能保健食品中违禁添加的降糖类药物[J].食品安全质量检测学报,2013,4(3):722-729.LIU Bo,WU Ting-ting,HOU Yu-lan,et al.Rapid determination of sugar-reducing medicine in health food by DCBI-MS method[J].Journal of Food Safety and Quality,2013,4(3):722-729.
 贾华,尹瑞林,钟旭,等.分子印迹复合膜对降糖药的拉曼光谱快速检测[J].高等学校化学学报,2016,37(2):239-245.JIA Hua,YIN Rui-lin,ZHONG Xu,et al.Anti-diabetic drugs detection by raman spectrometry with molecular imprinted composite membrane[J].Chemical Journal of Chinese Universities,2016,37(2):239-245.
 张中湖,李军,谢强胜,等.TLC-SERS高通量筛查中成药与保健食品中添加的降糖化学物质[J].药物分析杂志,2019,39(3):467-476.ZHANG Zhong-hu,LI Jun,XIE Qiang-sheng,et al.High-throughput screening of the hypoglycemic chemicals added in chinese patent medicines and health foods by TLC-SERS[J].Chinese Journal of Pharmaceutical Analysis,2019,39(3):467-476.
 李荣,卫星华,董靖.HPLC-DAD法测定中成药及保健食品中非法添加16种降糖类化学药物的研究[J].辽宁中医杂志,2018,45(5):1 022-1 024.LI Rong,WEI Xing-hua,DONG Jing.Determination of 16 anti-diabetic agents illegally added in traditional chinese medicines and health food by HPLC-DAD[J].Liaoning Journal of Traditional Chinese Medicine,2018,45(5):1 022-1 024.
 KIM N S,KIM K Y,YOO G J,et al.Determination of 26 anti-diabetic compounds in dietary supplements using a validated UPLC method[J].Food Additives & Contaminants:Part A,2018,35(3):387-394.
 ZHOU C,TANG B,XI C,et al.Simultaneous determination of seven sulfonylurea-type oral anti-diabetic agents in adulterated dietary supplements and traditional chinese medicines by ultraperformance liquid chromatography-tandem mass spectrometry[J].Spectroscopy Letters,2015,48(3):163-169.
 安莹,周颖,季剑波,等.辅助降糖胶囊中3种双胍类物质的快速筛查[J].食品与机械,2020,36(12):49-52.AN Ying,ZHOU Ying,JI Jian-bo,et al.Rapid screening of three kinds of guanidine contraband in auxiliary sugar reduction capsule[J].Food & Machinery,2020,36(12):49-52.
 林黛琴,万承波,曾春,等.高效液相色谱—串联质谱法快速测定保健食品中非法添加的9种降糖药物[J].南昌大学学报(理科版),2020,44(4):370-374.LIN Dai-qin,WAN Cheng-bo,ZENG Chun,et al.Rapid determination of nine anti-diabetic chemicals in health care products by HPLC-MS/MS[J].Journal of Nanchang University(Natural Science),2020,44(4):370-374.
 朱青,曹美萍,张继春,等.超高效液相色谱—串联质谱法检测多基质保健食品中27种非法添加降糖类化合物[J].食品安全质量检测学报,2021,12(11):4 480-4 491.ZHU Qing,CAO Mei-ping,ZHANG Ji-chun,et al.Determination of 27 kinds of anti-diabetic compounds illegally in different kinds of health food by ultra-performance liquid chromatographytandem mass spectrometry[J].Journal of Food Safety and Quality,2021,12(11):4 480-4 491.
 韩智,龚蕾,王会霞,等.轨道离子阱快速筛查及定量分析保健食品中73种非法添加成分[J].食品与机械,2019,35(7):74-79,116.HAN Zhi,GONG Lei,WANG Hui-xia,et al.Rapid screening and quantitative analysis of 73 kinds of chemicals illegally added in the healthy foods by orbitrap mass spectrometry[J].Food & Machinery,2019,35(7):74-79,116.
 马静,李浩.液相色谱—串联质谱法测定人血浆中利格列汀的浓度[J].中国临床药理学杂志,2018,34(20):2 435-2 437.MA Jing,LI Hao.Determination of linagliptin in human plasma by HPLC-MS/MS[J].The Chinese Journal of Clinical Pharmacology,2018,34(20):2 435-2 437.
 LIU Y,SONG L,YAO X,et al.A high-performance liquid chromatography-tandem mass spectrometry method for simultaneous determination of imigliptin,its five metabolites and alogliptin in human plasma and urine and its application to a multiple-dose pharmacokinetic study[J].Biomedical Chromatography,2018,32(11):e4324.
 PENG Y,CHANG Q,YANG N,et al.Quantitative determination of metformin,saxagliptin and 5-hydroxy saxagliptin simultaneously by hydrophilic interaction liquid chromatography-electrospray ionization mass spectrometry and its application to a bioequivalence study with a single-pill combination in human[J].Journal of Chromatography B,2018,1 081/1 082:109-117.
 ABOU-OMAR M N,KENAWY M,YOUSSEF A O,et al.Validation of a novel UPLC-MS/MS Method for estimation of Metformin and Empagliflozin simultaneously in human plasma using freezing lipid precipitation approach and its application to pharmacokinetic study[J].Journal of Pharmaceutical and Biomedical Analysis,2021,200:114078.
 杨庆懿,杨柳,王凯,等.超高效液相色谱—串联质谱法同时测定保健食品中15种非法添加降糖化学药物[J].食品安全质量检测学报,2019,10(7):2 038-2 042.YANG Qing-yi,YANG Liu,WANG Kai,et al.Simultaneous determination of 15 kinds of illegally added hypoglycemic chemicals in health foods by ultra performance liquid chromatography-tandem mass spectrometry[J].Journal of Food Safety and Quality,2019,10(7):2 038-2 042.
 陈鹏.气质联用和液质联用中基质效应研究进展[J].天津药学,2020,32(4):67-72.CHEN Peng.Study on matrix effect in GC-MS and LC-MS[J].Tianjin Pharmacy,2020,32(4):67-72.