超高效液相色谱-四极杆/飞行时间高分辨质谱法用于保健食品中6种非法添加降脂类药物的快速筛查与定量分析
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摘要
目的建立超高效液相色谱-四极杆/飞行时间高分辨质谱法快速测定保健食品中烟酸、辛伐他汀、美伐他汀、洛伐他汀、去羟基洛伐他汀和洛伐他汀羟酸钠盐的方法。方法采用Waters ACQUITY UPLC HSS T3色谱柱,以0.1%甲酸(V:V)-甲醇为流动相梯度洗脱,流速0.3 mL/min,柱温35℃,在电喷雾离子源、正离子模式下,以多反应监测方式检测6种非法添加降脂类药物。结果 6种化合物标准品溶液浓度和检测响应的线性关系良好,其相关系数r均大于0.998;检出限在0.56～50.10ng/mL,定量限在1.67～100.20ng/mL,方法准确度、精密度、重复性均可满足要求。结论该方法简单、准确、高效,可用于保健食品中6种降脂类药物的快速筛查和定量测定。
Objective To establish a method for determination of nicotinic acid, simvastatin, mevastatin,lovastatin, dehydro lovastatin and lovastatin hydroxy acid sodium salt in health food by ultra performance liquid chromatography tandem quadrupole/time-of-flight high resolution mass spectrometry(UPLC/Q-TOF-HRMS).Methods A Waters ACQUITY UPLC HSS T3 chromatographic column was used with the mobile phase of 0.1%(V:V) formic acid aqueous solution-methanol for gradient elution, the flow rate was 0.3 mL/min, and the column temperature was 35 ℃. Electrospray ionization(ESI) source was applied and operated in positive mode, 6 lipid-lowering drugs illegally added in health food were detected by multiple reactions monitoring(MRM) mode.Results Six lipid-lowering drugs had good linear relationships, and the correlation coefficients were greater than 0.998. The limits of detection of 6 lipid-lowering drugs were 0.56-50.10 ng/mL, and the limits of quantitation were 1.67-100.20 ng/mL. Precision, accuracy and repeatability was all satisfied. Conclusion This method is simple,accurate and efficient, which is suitable for rapid screening and quantitative analysis of 6 illegally added drugs in lipid-lowering health foods.
Objective To establish a method for determination of nicotinic acid, simvastatin, mevastatin,lovastatin, dehydro lovastatin and lovastatin hydroxy acid sodium salt in health food by ultra performance liquid chromatography tandem quadrupole/time-of-flight high resolution mass spectrometry(UPLC/Q-TOF-HRMS).Methods A Waters ACQUITY UPLC HSS T3 chromatographic column was used with the mobile phase of 0.1%(V:V) formic acid aqueous solution-methanol for gradient elution, the flow rate was 0.3 mL/min, and the column temperature was 35 ℃. Electrospray ionization(ESI) source was applied and operated in positive mode, 6 lipid-lowering drugs illegally added in health food were detected by multiple reactions monitoring(MRM) mode.Results Six lipid-lowering drugs had good linear relationships, and the correlation coefficients were greater than 0.998. The limits of detection of 6 lipid-lowering drugs were 0.56-50.10 ng/mL, and the limits of quantitation were 1.67-100.20 ng/mL. Precision, accuracy and repeatability was all satisfied. Conclusion This method is simple,accurate and efficient, which is suitable for rapid screening and quantitative analysis of 6 illegally added drugs in lipid-lowering health foods.
引文
[1]宁霄,张伟清,王钢力,等.保健食品中非法添加药物的检测现状及筛查策略研究[J].食品安全质量检测学报,2015,6(5):1876-1882.Ning X,Zhang WQ,Wang GL,et al.Detection status and screening strategy of illegally added drugs in healthy food[J].J Food Saf Qual,2015,6(5):1876-1882.
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[4]王铁松,仝禹,郑洁,等.薄层色谱法快速筛查降脂、降压、止咳平喘类中药制剂中的29种添加化学药物[J].中国药学杂志,2010,45(11):857-861.Wang TS,Tong Y,Zheng J,et al.Detection of 29 adulterations in lipid-regulating,antihypertensive,antitussive and antiasthmatic herbal remedies by TLC[J].Chin Pharm J,2010,45(11):857-861.
[5]孙亮,张蓉,邬国庆,等.高效液相色谱法同时测定保健食品中9种非法添加降脂类药物[J].食品安全质量检测学报,2016,7(8):3098-3102.Sun L,Zhang R,Wu GQ,et al.Simultaneous determination of 9 kinds of lipid lowering drugs illegally added in health food by high performance liquid chromatography[J].J Food Saf Qual,2016,7(8):3098-3102.
[6]邓鸣,朱斌,尹利辉.中成药及保健食品中非法添加调血脂类药物的HPLC快速检测方法研究,[J].药物分析杂志,2016,36(9):1639-1647.Deng M,Zhu B,Yin LH.Rapid HPLC testing method for lipid-regulating drugs illegally added in traditional Chinese medicines and health food[J].Chin J Pharm Anal,2016,36(9):1639-1647.
[7]胡青,崔益泠,张甦,等.降血脂和降血糖类中药及保健食品中违禁添加17种化学药物的液相色谱-离子阱质谱定性检测[J].中国医药工业杂志,2009,40(2):124-127.Hu Q,Cui YL,Zhang S,et al.Detection 17 chemical drugs illegally added in traditional Chinese medicine for reducing blood fat and lowering blood sugar and health food by LC-MSn trap[J].Chin J Pharm,2009,40(2):124-127.
[8]宫旭,芦丽,冯有龙,等.UPLC-MS/MS法测定减肥降脂通便三类保健食品中添加的37种药物[J].药物分析杂志,2016,36(5):918-928.Gong X,Lu L,Feng YL,et al.Determination of 37 drugs illegally added in weight-losing lipid-lowering and laxative health foods by UPLC-MS/MS[J].Chin J Pharm Anal,2016,36(5):918-928.
[9]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):594-600.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 JChromatogr,2017,35(6):594-600.
[10]于泓,胡青,张甦,等.超高效液相色谱-四级杆-飞行时间串联质谱法检测中药及保健食品中21种非法添加的降脂类药物[J].食品安全质量检测学报,2016,7(7):2704-2709.Yu H,Hu Q,Zhang S,et al.Determination of 21 kinds of lipid-lowering drugs in herbal products and dietary supplements by ultra performance liquid chromatography/quadrupole-time-of-flight mass spectrometry[J].JFood Saf Qual,2016,7(7):2704-2709.
[11]姜树银,郭常川,石峰,等.Q-Orbitrap高分辨质谱用于降血脂类中成药和保健食品中非法添加物的快速筛查、鉴定和定量[J].药物分析杂志,2015,35(8):1447-1452.Jiang SY,Guo CC,Shi F,et al.Application of Q-Orbitrap high resolution mass spectrometry to the detection of illegal adulterated antihyperlipidemics in herbal medicines and dietary supplements[J].Chin J Pharm Anal,2015,35(8):1447-1452.
[12]钮正睿,王聪,丁宏,等.超高效液相色谱-四极杆/飞行时间高分辨质谱测定保健食品及其原料中洛伐他汀及类似物的含量[J].食品安全质量检测学报,2017,8(7):2563-2570.Niu ZR,Wang C,Ding H,et al.Simultaneous determination of lovastatin and its analogues in health food and raw materials by ultra performance liquid chromatography tandem quadrupole/time-of-flight high resolution mass spectrometry[J].J Food Saf Qual,2017,8(7):2563-2570.
[13]丁博,王志元,谢建军,等.QuEChERS前处理技术联合液相色谱-四极杆飞行时间质谱法检测保健食品中24种违禁降血糖、降血压和降血脂药物[J].色谱,2016,34(6):583-590.Ding B,Wang ZY,Xie JJ,et al.Determination of 24 antihyperglycemic,antihypertensive and antihyperlipidemic drugs illegally added in health food samples by liquid chromatography-quadrupole-time of flight mass spectrometry[J].Chin J Chromatogr,2016,34(6):583-590.
[14]郝刚,顾炳仁.UPLC-MS/MS检测降血脂类保健食品中违法添加物[J].中国执业药师,2014,11(7):20-23,56.Hao G,Gu BR.Rapid identification of illegal additives in lipid lowering health foods by UPLC-MS/MS[J].China Licensed Pharm,2014,11(7):20-23,56.
[2]孙晶,张中湖,王维剑.降脂减肥等七类中成药非法添加西药情况研究[J].药学研究,2013,32(3):174-176.Sun J,Zhang ZH,Wang WJ.Study on illegal addition of western medicine to 7 kinds of Chinese formulated products[J].J Pharm Res,2013,32(3):174-176.
[3]张喆,高青,车宝泉,等.中药和保健食品中非法添加降脂类药物的检测方法研究[J].药物分析杂志,2008,25(12):2069-2072.Zhang Z,Gao Q,Che BQ,et al.Study on the detection method of lipid-lowering drugs illegally added in traditional Chinese medicine and health food[J].Chin J Pharm Anal,2008,25(12):2069-2072.
[4]王铁松,仝禹,郑洁,等.薄层色谱法快速筛查降脂、降压、止咳平喘类中药制剂中的29种添加化学药物[J].中国药学杂志,2010,45(11):857-861.Wang TS,Tong Y,Zheng J,et al.Detection of 29 adulterations in lipid-regulating,antihypertensive,antitussive and antiasthmatic herbal remedies by TLC[J].Chin Pharm J,2010,45(11):857-861.
[5]孙亮,张蓉,邬国庆,等.高效液相色谱法同时测定保健食品中9种非法添加降脂类药物[J].食品安全质量检测学报,2016,7(8):3098-3102.Sun L,Zhang R,Wu GQ,et al.Simultaneous determination of 9 kinds of lipid lowering drugs illegally added in health food by high performance liquid chromatography[J].J Food Saf Qual,2016,7(8):3098-3102.
[6]邓鸣,朱斌,尹利辉.中成药及保健食品中非法添加调血脂类药物的HPLC快速检测方法研究,[J].药物分析杂志,2016,36(9):1639-1647.Deng M,Zhu B,Yin LH.Rapid HPLC testing method for lipid-regulating drugs illegally added in traditional Chinese medicines and health food[J].Chin J Pharm Anal,2016,36(9):1639-1647.
[7]胡青,崔益泠,张甦,等.降血脂和降血糖类中药及保健食品中违禁添加17种化学药物的液相色谱-离子阱质谱定性检测[J].中国医药工业杂志,2009,40(2):124-127.Hu Q,Cui YL,Zhang S,et al.Detection 17 chemical drugs illegally added in traditional Chinese medicine for reducing blood fat and lowering blood sugar and health food by LC-MSn trap[J].Chin J Pharm,2009,40(2):124-127.
[8]宫旭,芦丽,冯有龙,等.UPLC-MS/MS法测定减肥降脂通便三类保健食品中添加的37种药物[J].药物分析杂志,2016,36(5):918-928.Gong X,Lu L,Feng YL,et al.Determination of 37 drugs illegally added in weight-losing lipid-lowering and laxative health foods by UPLC-MS/MS[J].Chin J Pharm Anal,2016,36(5):918-928.
[9]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):594-600.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 JChromatogr,2017,35(6):594-600.
[10]于泓,胡青,张甦,等.超高效液相色谱-四级杆-飞行时间串联质谱法检测中药及保健食品中21种非法添加的降脂类药物[J].食品安全质量检测学报,2016,7(7):2704-2709.Yu H,Hu Q,Zhang S,et al.Determination of 21 kinds of lipid-lowering drugs in herbal products and dietary supplements by ultra performance liquid chromatography/quadrupole-time-of-flight mass spectrometry[J].JFood Saf Qual,2016,7(7):2704-2709.
[11]姜树银,郭常川,石峰,等.Q-Orbitrap高分辨质谱用于降血脂类中成药和保健食品中非法添加物的快速筛查、鉴定和定量[J].药物分析杂志,2015,35(8):1447-1452.Jiang SY,Guo CC,Shi F,et al.Application of Q-Orbitrap high resolution mass spectrometry to the detection of illegal adulterated antihyperlipidemics in herbal medicines and dietary supplements[J].Chin J Pharm Anal,2015,35(8):1447-1452.
[12]钮正睿,王聪,丁宏,等.超高效液相色谱-四极杆/飞行时间高分辨质谱测定保健食品及其原料中洛伐他汀及类似物的含量[J].食品安全质量检测学报,2017,8(7):2563-2570.Niu ZR,Wang C,Ding H,et al.Simultaneous determination of lovastatin and its analogues in health food and raw materials by ultra performance liquid chromatography tandem quadrupole/time-of-flight high resolution mass spectrometry[J].J Food Saf Qual,2017,8(7):2563-2570.
[13]丁博,王志元,谢建军,等.QuEChERS前处理技术联合液相色谱-四极杆飞行时间质谱法检测保健食品中24种违禁降血糖、降血压和降血脂药物[J].色谱,2016,34(6):583-590.Ding B,Wang ZY,Xie JJ,et al.Determination of 24 antihyperglycemic,antihypertensive and antihyperlipidemic drugs illegally added in health food samples by liquid chromatography-quadrupole-time of flight mass spectrometry[J].Chin J Chromatogr,2016,34(6):583-590.
[14]郝刚,顾炳仁.UPLC-MS/MS检测降血脂类保健食品中违法添加物[J].中国执业药师,2014,11(7):20-23,56.Hao G,Gu BR.Rapid identification of illegal additives in lipid lowering health foods by UPLC-MS/MS[J].China Licensed Pharm,2014,11(7):20-23,56.