| 超高效液相色谱-串联质谱法同时快速检测微量血清中6种脂溶性维生素 |
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| 引用本文： | 李雪梅,吴慧慧,陈竞,赵盼,唐玉菲.超高效液相色谱-串联质谱法同时快速检测微量血清中6种脂溶性维生素[J].现代预防医学,2022,0(7):1297-1302. |
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| 作者姓名： | 李雪梅 吴慧慧 陈竞 赵盼 唐玉菲 |
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| 作者单位： | 1.安徽省第二人民医院（安徽省职业病防治院）职业卫生实验室，安徽 合肥 230041；2.中国疾病预防控制中心营养与健康所，国家卫生健康委员会微量元素与营养重点实验室 |
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| 摘 要： | 目的 建立超高效液相色谱-串联质谱法（UPLC-MS/MS）同时快速检测微量血清中维生素A、维生素D（25-OH-VD2 、25-OH-VD3 ）、维生素E（α-、β-和γ-生育酚）的方法。方法 血清中脂溶性维生素经甲醇-乙腈（50:50, v/v)沉淀蛋白、正己烷萃取，以Phenomenex Kinetex F5色谱柱为分离柱，2.5 mmol/L甲酸铵-0.1%甲酸水溶液和甲醇为流动相，梯度洗脱，电喷雾电离（ESI+ ）、多反应监测（MRM）模式下检测，同位素内标法定量。结果 血清中6种脂溶性维生素线性范围内线性关系良好，相关系数 r >0.995；6种脂溶性维生素的检测限为0.20~1.25 ng/ml，定量限为0.39~3.88 ng/ml；加标回收率为86.6%~107.7%，日内精密度<9.6%，日间精密度<9.3%。NIST标准参照品SRM 968f验证方法准确度，结果偏差均在5%以内。结论 本方法准确度高、重现性好、用血量少，适于婴幼儿等采血困难者微量血样中多种脂溶性维生素的同时快速检测。
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| 关 键 词： | 脂溶性维生素 血清 超高效液相色谱-串联质谱法（UPLC-MS/MS） |
An ultra-performance liquid chromatography-tandem mass spectrometry method for simultaneous and rapid detection of six fat-soluble vitamins in small volumes of serum |
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| LI Xue-mei,WU Hui-hui,CHEN Jing,ZHAO Pan,TANG Yu-fei.An ultra-performance liquid chromatography-tandem mass spectrometry method for simultaneous and rapid detection of six fat-soluble vitamins in small volumes of serum[J].Modern Preventive Medicine,2022,0(7):1297-1302. |
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| Authors: | LI Xue-mei WU Hui-hui CHEN Jing ZHAO Pan TANG Yu-fei |
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| Affiliation: | *Occupational Health Laboratory, Anhui NO.2 Provincial People’s Hospital(Anhui Prevention and Treatment Center for Occupational Disease), Hefei, Anhui 230041, China |
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| Abstract: | Objective To establish an ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the rapid and simultaneous detection of six fat-soluble vitamins including vitamin A (Retinol) and vitamin D (25-OH-VD2 , 25-OH-VD3 ), vitamin E (α-tocopherol, β-tocopherol, and γ-tocopherol) in small volumes of serum. Methods The serum samples were precipitated with methanol-acetonitrile （50:50, v/v), extracted with n-hexane. The separation of the target analytes was performed on a Phenomenex Kinetex F5 column（100 mm×2.1 mm，2.6 μm）with methanol and 2.5 mmol/L ammonium formate -0.1% formic acid aqueous solution as mobile phases under gradient elution. The detection was in the multiple reaction monitoring (MRM) mode with electrospray ionization (ESI) under positive conditions. The quantifications were based on the isotope internal standard method. Results The method showed good linearity within the linear range, with the correlation coefficients ( r )>0.995. The detection limits and the quantification limits of the six fat-soluble vitamins were 0.20-1.25 ng/ml and 0.39-3.88 ng/ml, respectively. The recoveries of the method spiked at the three levels were 86.6%-107.7%, with the intraday precision less than 9.6% and inter-day precision less than 9.3%, respectively. The accuracy of the method was assessed using the standard reference material (NIST SRM 968f), with the deviations all less than 5%. Conclusion The method is accurate, reproducible, and sample-saving, and it applies to the simultaneous and rapid detection of 6 fat-soluble vitamins in the trace serum sample, especially for infants and young children who have difficulty in blood collection. |
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| Keywords: | Fat-soluble vitamins Serum Ultra Performance Liquid Chromatography-tandem Mass Spectrometry（UPLC-MS/MS） |
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