高效液相色谱-串联质谱法测定降压类保健食品中5种α-受体阻断剂类非法添加药物的含量
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摘要
目的 建立高效液相色谱-串联质谱(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)法检测降压类保健食品中5种α-受体阻断剂含量的检测斱法。方法 样品经甲醇提取,残留物经Waters Sunfire C_18 (100 mm×2.1 mm, 5μm)色谱柱分离,以0.1%甲酸水溶液-0.1%甲酸乙腈溶液为流动相梯度洗脱,流速为0.3 mL/min,采用多反应监测正离子模式,定性和定量测定降压类保健食品中酚妥拉明、妥拉唑林、哌唑嗪、特拉唑嗪和育亨宾等5种α-受体阻断剂。结果 5种α-受体阻断剂分别在0.5～160μg/L浓度范围内呈现良好的线性关系,相关系数均大于0.993;酚妥拉明和哌唑嗪斱法的检出限为5μg/kg,定量限为10μg/kg;特拉唑嗪和育亨宾的检出限为2μg/kg,定量限为5μg/kg;妥拉唑林的检出限为15μg/kg,定量限为40μg/kg;添加水平分别为10～100、5～50、40～400μg/kg时,样品平均回收率为81.6%～113.5%,相对标准偏差为0.69%～4.80%(n=5)。结论 该斱法简便、快捷、准确、灵敏度高,适用于降压类保健食品中非法添加的酚妥拉明、妥拉唑林、哌唑嗪、特拉唑嗪及育亨宾等5种α-受体阻断剂的快速检测。
Objective To establish a method for determination of 5 kinds of α-receptor antagonists residues in antihypertensive health foods by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Methods The sample was extracted with methanol, and the residue was separated on a Waters Sunfire C_18(100 mm× 2.1 mm, 5 μm) column. The gradient was eluted with 0.1% aqueous formic acid-0.1% formic acid in acetonitrile as a mobile phase gradient at a flow rate of 0.3 mL/min. Five kinds of α-receptor antagonists such as phentolamine,tolazoline, prazosin, terazosin and yohimbine in antihypertensive health foods were qualitatively and quantitatively determined with positive ion mode with multiple reactions. Results The 5 α-receptor antagonists showed good linear relationships in the range of 0.5-160 μg/L, and the correlation coefficients were greater than 0.993. The detection limits of phentolamine and prazosin were 5 μg/kg, and the limits of quantification were 10 μg/kg. The detection limits of terazosin and yohimbine were 2 μg/kg, and the limits of quantification were 5 μg/kg. The detection limit of tolazoline was 15 μg/kg, and the limit of quantification was 40 μg/kg. When the addition levels were 10-100,5-50, and 40-400 μg/kg, the average recoveries of samples were 81.6%-113.5%, and the relative standard deviations were 0.69%-4.80%(n=5). Conclusion The method is simple, rapid, accurate and sensitive, which is suitable for rapid detection of 5 kinds of α-receptor antagonists such as phentolamine, tolazoline, prazosin, terazosin and yohimbine illegally added in antihypertensive health food.
Objective To establish a method for determination of 5 kinds of α-receptor antagonists residues in antihypertensive health foods by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Methods The sample was extracted with methanol, and the residue was separated on a Waters Sunfire C_18(100 mm× 2.1 mm, 5 μm) column. The gradient was eluted with 0.1% aqueous formic acid-0.1% formic acid in acetonitrile as a mobile phase gradient at a flow rate of 0.3 mL/min. Five kinds of α-receptor antagonists such as phentolamine,tolazoline, prazosin, terazosin and yohimbine in antihypertensive health foods were qualitatively and quantitatively determined with positive ion mode with multiple reactions. Results The 5 α-receptor antagonists showed good linear relationships in the range of 0.5-160 μg/L, and the correlation coefficients were greater than 0.993. The detection limits of phentolamine and prazosin were 5 μg/kg, and the limits of quantification were 10 μg/kg. The detection limits of terazosin and yohimbine were 2 μg/kg, and the limits of quantification were 5 μg/kg. The detection limit of tolazoline was 15 μg/kg, and the limit of quantification was 40 μg/kg. When the addition levels were 10-100,5-50, and 40-400 μg/kg, the average recoveries of samples were 81.6%-113.5%, and the relative standard deviations were 0.69%-4.80%(n=5). Conclusion The method is simple, rapid, accurate and sensitive, which is suitable for rapid detection of 5 kinds of α-receptor antagonists such as phentolamine, tolazoline, prazosin, terazosin and yohimbine illegally added in antihypertensive health food.
引文
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[13]刘畅,夏晶,胡青,等.LC/MS(n)法检测补肾壮阳药类中成药和保健食品中非法添加5种性功能类化学药品[J].中成药,2009,31(9):1371-1374.Liu C,Xia J,Hu Q,et al.Determination of 5 aphrodisiacs illegal adulterated into chinese proprietary medicine by LC/MS(n)trap[J].Chin Trad Patent Med,2009,31(9):1371-1374.
[14]褚滢倩,陈溪,崔妍,等.色谱质谱分析技术在快速筛查检测领域的研究进展[J].食品安全质量检测学报,2018,9(24):6355-6361.Zhu YQ,Chen X,Cui Y,et al.Research process of chromatographic mass spectrometry in the field of rapid screening and detection[J].J Food Saf Qual,2018,9(24):6355-6361.
[15]徐硕,金鹏飞,徐文峰,等.补肾壮阳类药品中非法添加化学药物检测技术的研究进展[J].西北药学杂质,2017,32(5):677-680.Xu S,Jin PF,Xu W,et al.Research advance on analytical technologies of illegally adulterated chemical substance in medicine for invigorants[J].Northwest Pharm J,2017,32(5):677-680.
[16]张园,闵春艳,郝刚,等.保健食品中非法添加化学药物的检测斱法[J].中国执业药师,2014,11(7):35-39.Zhang Y,Min CY,Hao G,et al.Screening method for illegally added chemical in health foods[J].China Licensed Pharm,2014,11(7):35-39.
[2]张丼霞.α-受体阻断药在治疗良性前列腺增生中的地位和作用[J].中国药师,2002,5(1):51-52.Zhang LX.Role ofα-receptor antagonists in the treatment of benign prostatic hypertrophy[J].China Pharm,2002,5(1):51-52.
[3]徐文峰,徐硕,金鹏飞.辅助降血压类中成药和保健食品中非法添加化学药物检测技术的研究进展[J].中国医药导报,2016,12(31):61-64.Xu WF,Xu S,Jin PF.Research process on detection technologies of illegal adulterated chemical substances in antihypertensive traditional Chinses medicines and dietary supplements[J].Chin Med Herald,2016,12(31):61-64.
[4]吴公平,雷玉萍,黎银波,等.辅助降压类保健品中非法添加化学药品的快速筛选斱法[J].中国药业,2010,19(14):42-43Wu GP,Lei YP,Li YB,et al.TLC determination of multiple-component illegally added in antihypertensive health care product[J].Chin Pharm,2010,19(14):42-43.
[5]翁水旺,刘解民.紫外分光光度法测定甲磺酸酚妥拉明分散片的含量[J].解放军药学学报,2000,16(2):107-109.Weng SW,Liu JM.Determination of dispersible Phentolamine mesylate tablets by UV spectrophotometry[J].Pharm J Chin PLA,2000,16(2):107-109.
[6]刘兊江,李素娣.荧光法测定盐酸特拉唑嗪胶囊的含量[J].中国现代应用药学杂志,2005,22(6):487-489.Liu KJ,Li SD.Determination of terazosin hydrochloride capsules by fluorescence spectroscopy[J].Chin J Mod Appl Pharm,2005,22(6):487-489.
[7]季任东,赵志敏,张吉华,等.基于牛血清白蛋白荧光探针的盐酸特拉唑嗪含量测定[J].发光学报,2014,35(8):1014-1017.Ji RD,Zhao ZM,Zhang JH J,et al.Determination of terazosin hydrochloride tablets by using bovine serum albumin as fluorescent probe[J].Chin J Lumin,2014,35(8):1014-1017.
[8]陈琴华,李鹏,何婧.非水毛细管电泳法快速测定盐酸哌唑嗪片中主药的含量[J].中国药房,2009,20(34):2705-2706.Chen QH,Li P,He J.Rapid determination of prazosin in prazosin hydrochloride tablets by non-aqueous capillary electrophoresis[J].China Pharm,2009,20(34):2705-2706.
[9]牛长群,任雷鸣.3种新型α1-受体阻断剂的高效毛细管电泳手性分离[J].药学学报,2000,35(6):451-453.Niu CQ,Ren LM.Chiral separation of three new antagonists of alpha1-adrenoceptors by capillary electrophoresis[J].Acta Pharm Sin,2000,35(6):451-453.
[10]陈林,温家欣,齐春艳,等.降压类中成药及保健食品中21种非法添加化学药物的快速检测与确证斱法研究[J].分析测试学报,2016,35(8):937-942.Chen L,Wen JX,Qi CY,et al.Rapid determination and confirmation 21illegal chemical drugs in antihypertension traditional Chinese medicine and healthy food[J].J Instrum Anal,2016,35(8):937-942.
[11]于转转,余以兵,武爱国,等.HPLC法测定盐酸哌唑嗪消旋山莨菪碱片中盐酸哌唑嗪及消旋山莨菪碱的含量[J].解放军药学学报,2014,30(6):519-521.Yu ZZ,Yu YB,Wu AG,et al.Determination of content of raceanisodamine and prazosin hydrochloride in prazosin hydrochloride raceanisodamine tablets by HPLC[J].Pharm J Chin PLA,2014,30(6):519-521.
[12]魏志雄,刘丹丹.LC-MS/MS法检测降压类中成药及保健品中非法添加的7种化学药物[J].亚太传统医药,2014,10(11):12-14.Wei ZX,Liu DD.Determination of seven chemical medicines in antihypertensive traditional Chinese medicine and health foods by LC-MS/MS[J].Asia Pacif Trad Med,2014,10(11):12-14.
[13]刘畅,夏晶,胡青,等.LC/MS(n)法检测补肾壮阳药类中成药和保健食品中非法添加5种性功能类化学药品[J].中成药,2009,31(9):1371-1374.Liu C,Xia J,Hu Q,et al.Determination of 5 aphrodisiacs illegal adulterated into chinese proprietary medicine by LC/MS(n)trap[J].Chin Trad Patent Med,2009,31(9):1371-1374.
[14]褚滢倩,陈溪,崔妍,等.色谱质谱分析技术在快速筛查检测领域的研究进展[J].食品安全质量检测学报,2018,9(24):6355-6361.Zhu YQ,Chen X,Cui Y,et al.Research process of chromatographic mass spectrometry in the field of rapid screening and detection[J].J Food Saf Qual,2018,9(24):6355-6361.
[15]徐硕,金鹏飞,徐文峰,等.补肾壮阳类药品中非法添加化学药物检测技术的研究进展[J].西北药学杂质,2017,32(5):677-680.Xu S,Jin PF,Xu W,et al.Research advance on analytical technologies of illegally adulterated chemical substance in medicine for invigorants[J].Northwest Pharm J,2017,32(5):677-680.
[16]张园,闵春艳,郝刚,等.保健食品中非法添加化学药物的检测斱法[J].中国执业药师,2014,11(7):35-39.Zhang Y,Min CY,Hao G,et al.Screening method for illegally added chemical in health foods[J].China Licensed Pharm,2014,11(7):35-39.