UPLC-MS/MS同时测定保健食品中洛伐他汀及其类似物
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摘要
建立超高效液相色谱—串联质谱法同时检测保健食品中5种降脂类药物(洛伐他汀、辛伐他汀、美伐他汀、去羟基洛伐他汀、洛伐他汀羟酸钠盐)的方法,样品以甲醇超声提取后,用Waters Acquity HSS T3色谱柱分离,乙腈—0.1%甲酸水溶液梯度洗脱,流速为0.3mL/min,电喷雾离子源正负离子同时扫描,多反应监测(MRM)方式检测,外标法定量。结果表明:该条件下5min内可准确地定性定量分析5种化合物,分离度好,检出限为15μg/kg,定量限为50μg/kg,加标回收率为94.6%～105.7%。用此方法检测17批市售降血脂保健食品,其中1批次样品测出洛伐他汀、洛伐他汀羟酸钠盐、去羟基洛伐他汀。该方法简便、快速、灵敏、准确,适合于保健食品中的洛伐他汀及其类似物的快速测定。
A ultra-high performance liquid chromatographytandem mass spectrometric(UPLC-MS/MS)assay method has been developed and fully validated for the simultaneous quantification of lovastatin,simvastatin,mevastatin,lovastatin sodium hydroxide,dehydro lovastatin.The samples were extracted with methanol and separated on a Waters Acquity HSS T3 column.The mobile phase consisting of 0.1%aqueous formic acid solution and acetonitrile using gradient elution at a flow rate of0.3 mL/min.The positive and negative ions were scanned simultaneously.The multiple reaction monitoring(MRM)mode was used for detection.The results showed that the five compounds were separated well within five minutes.The limits of detection and the limits of quantification were 15μg/kg and 50μg/kg,respectively.The recoveries were between 94.6% ～105.7%,and the relative standard deviation of the methods were lower than10%.17 batches of hypolipidemic health food were tested by this method,lovastatin,lovastatin sodium hydroxide salt and dehydro lovastatin were detected in one batch of samples.The method was simple,rapid,sensitive and accurate,and it was suitable for the rapid determination of lovastatin and its analogues in functional foods.
A ultra-high performance liquid chromatographytandem mass spectrometric(UPLC-MS/MS)assay method has been developed and fully validated for the simultaneous quantification of lovastatin,simvastatin,mevastatin,lovastatin sodium hydroxide,dehydro lovastatin.The samples were extracted with methanol and separated on a Waters Acquity HSS T3 column.The mobile phase consisting of 0.1%aqueous formic acid solution and acetonitrile using gradient elution at a flow rate of0.3 mL/min.The positive and negative ions were scanned simultaneously.The multiple reaction monitoring(MRM)mode was used for detection.The results showed that the five compounds were separated well within five minutes.The limits of detection and the limits of quantification were 15μg/kg and 50μg/kg,respectively.The recoveries were between 94.6% ～105.7%,and the relative standard deviation of the methods were lower than10%.17 batches of hypolipidemic health food were tested by this method,lovastatin,lovastatin sodium hydroxide salt and dehydro lovastatin were detected in one batch of samples.The method was simple,rapid,sensitive and accurate,and it was suitable for the rapid determination of lovastatin and its analogues in functional foods.
引文
[1]张李伟,赵洪静,白鸿,等.中国保健食品法律法规体系发展与现状研究[J].中国食品卫生杂志,2008,20(3):232-235.
[2]张雪艳,王素珍.保健食品市场乱象成因分析及对策[J].中国食品药品监管,2018(8):49-53.
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[4]赵超群.液相色谱-串联质谱联用技术在测定食品中非法添加物的应用[D].杭州:浙江工业大学,2015:1-2.
[5]PATEL Misari,CHARMY Kothari.Critical review of statins:A bio-analytical perspective for therapeutic drug monitoring[J].Trends in Analytical Chemistry,2017,86:206-221.
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[11]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):3 098-3 102.
[12]HELI Sirén,LAURA Kaijanen,SINI Kaartinen,et al.Determination of statins by gas chromatography-EI/MRM-Tandem mass spectrometry:Fermentation of pine samples with Pleurotus ostreatus[J].Journal of Pharmaceutical and Biomedical Analysis,2014,94:196-202.
[13]GUO Meng-ran,ZHAO Long-shan,LI Mo,et al.Simultaneous determination of lovastatin and its metabolite lovastatin acid in rat plasma using UPLC-MS/MS with positive/negative ion-switching electrospray ionization:Application to a pharmacokinetic study of lovastatin nanosuspension[J].Journal of Chromatography B,2016,1 023:55-61.
[14]SRINIVASA Rao Polagani,NAGESWARA Rao Pilli,RA-MAKRISHNA Gajula,et al.Simultaneous determination of atorvastatin,metformin and glimepiride in human plasma by LC-MS/MS and its application to a human pharmacokinetic study[J].Journal of Pharmaceutical Analysis,2013,3(1):9-19.
[15]ASMA El-Zailik,LILY K Cheung,WANG Yang,et al.Simultaneous LC-MS/MS analysis of simvastatin,atorvastatin,rosuvastatin and their active metabolites for plasma samples of obese patients underwent gastric bypass surgery[J].Journal of Pharmaceutical and Biomedical Analysis,2019,164:258-267.
[16]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):2 704-2 709.
[17]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):2 563-2 570.
[2]张雪艳,王素珍.保健食品市场乱象成因分析及对策[J].中国食品药品监管,2018(8):49-53.
[3]王晶,李冰,奚茜,等.我国2003年以来注册的降脂保健茶的现状分析[J].中国食物与营养,2016,22(11):76-80.
[4]赵超群.液相色谱-串联质谱联用技术在测定食品中非法添加物的应用[D].杭州:浙江工业大学,2015:1-2.
[5]PATEL Misari,CHARMY Kothari.Critical review of statins:A bio-analytical perspective for therapeutic drug monitoring[J].Trends in Analytical Chemistry,2017,86:206-221.
[6]LIU Ai-mei,WU Qing-hua,GUO Jing-chao,et al.Statins:Adverse reactions,oxidative stress and metabolic interactions[J].Pharmacology and Therapeutics,2018,DOI:10.1016/j.pharmthera.2018.10.004.
[7]国家食品药品监督管理总局.《总局办公厅关于印发国家食品安全监督抽检实施细则(2018年版)的通知:食药监办食监三[2018]14号[EB/OL].(2018-01-18)[2019-01-24].http://samr.cfda.gov.cn/WS01/CL1605/223270.html.
[8]国家食品药品监督管理局.辅助降血脂类保健食品违法添加药物的检测方法:国食药监办许[2010]114号[EB/OL].(2010-04-27)[2019-01-24].http://www.instrument.com.cn/download/shtml/809955.shtml.
[9]国家市场监督管理局.全国食品保健食品欺诈和虚假宣传整治工作领导小组办公室发布《食品保健食品欺诈和虚假宣传整治问答》[EB/OL].(2018-10-19)[2019-01-24].http://samr.saic.gov.cn/xw/yw/xwfb/201810/t20181009_276222.Html.
[10]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.
[11]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):3 098-3 102.
[12]HELI Sirén,LAURA Kaijanen,SINI Kaartinen,et al.Determination of statins by gas chromatography-EI/MRM-Tandem mass spectrometry:Fermentation of pine samples with Pleurotus ostreatus[J].Journal of Pharmaceutical and Biomedical Analysis,2014,94:196-202.
[13]GUO Meng-ran,ZHAO Long-shan,LI Mo,et al.Simultaneous determination of lovastatin and its metabolite lovastatin acid in rat plasma using UPLC-MS/MS with positive/negative ion-switching electrospray ionization:Application to a pharmacokinetic study of lovastatin nanosuspension[J].Journal of Chromatography B,2016,1 023:55-61.
[14]SRINIVASA Rao Polagani,NAGESWARA Rao Pilli,RA-MAKRISHNA Gajula,et al.Simultaneous determination of atorvastatin,metformin and glimepiride in human plasma by LC-MS/MS and its application to a human pharmacokinetic study[J].Journal of Pharmaceutical Analysis,2013,3(1):9-19.
[15]ASMA El-Zailik,LILY K Cheung,WANG Yang,et al.Simultaneous LC-MS/MS analysis of simvastatin,atorvastatin,rosuvastatin and their active metabolites for plasma samples of obese patients underwent gastric bypass surgery[J].Journal of Pharmaceutical and Biomedical Analysis,2019,164:258-267.
[16]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):2 704-2 709.
[17]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):2 563-2 570.