液相色谱法测定保健酒中的西地那非和咖啡因
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摘要
建立了液相色谱法测定保健酒中西地那非和咖非因的含量。样品采用C18色谱柱梯度洗脱,波长为280nm,流动相为乙腈–0.1%磷酸溶液,柱温为30℃,采用二极管阵列检测器检测。西地那非和咖非因的质量浓度在5～200μg/mL范围内与色谱峰面积呈良好的线性关系,相关系数大于0.999,西地那非的检出限为0.32 mg/kg,咖啡因的检出限为0.17 mg/kg。测定结果的相对标准偏差为1.0%～3.0%(n=6),样品加标回收率为94.2%～98.7%。该方法操作简单、快速,结果准确,适用于保健酒中西地那非和咖啡因的同时测定。
A method for the determination of sildenafil and caffeine in health wine by liquid chromatography was established. The sample was eluted with C_(18) column gradient, the wavelength was 280 nm, the mobile phase was acetonitrile–0.1% phosphoric acid solution, the column temperature was 30℃, and the diode array detector was used. The mass concentration of sildenafil and caffeine had good linear relationship with the chromatographic peak area in the range of 5–200 μg/mL, the correlation coefficients were more than 0.999. The detection limit was 0.32 mg/kg for sildenafil, and 0.17 mg/kg for caffeine. The relative standard deviation of the detection results was 1.0%–3.0%(n=6), and the recoveries of sample were 94.2%–98.7%. The method is simple, rapid and accurate. It is suitable for simultaneous determination of sildenafil and caffeine in health wine.
A method for the determination of sildenafil and caffeine in health wine by liquid chromatography was established. The sample was eluted with C_(18) column gradient, the wavelength was 280 nm, the mobile phase was acetonitrile–0.1% phosphoric acid solution, the column temperature was 30℃, and the diode array detector was used. The mass concentration of sildenafil and caffeine had good linear relationship with the chromatographic peak area in the range of 5–200 μg/mL, the correlation coefficients were more than 0.999. The detection limit was 0.32 mg/kg for sildenafil, and 0.17 mg/kg for caffeine. The relative standard deviation of the detection results was 1.0%–3.0%(n=6), and the recoveries of sample were 94.2%–98.7%. The method is simple, rapid and accurate. It is suitable for simultaneous determination of sildenafil and caffeine in health wine.
引文
[1]郑佳,郭建军,罗惠波.保健酒发展及现状的思考[J].四川食品与发酵,2006,42(3):26-31.
[2]魏博通,陈力.我国保健酒市场发展的现状存在的问题与对策分析[J].商场现代化,2010(35):64-65.
[3]李安陵.关于保健酒的研发思考[J].酿酒,2009,36(5):87-90.
[4]陈玲,张炼,李文斌.不同剂量西地那非治疗新生儿肺动脉高压的疗效[J].华中科技大学学报(医学版),2012,41(2):210-213.
[5]王岩.西地那非联合硫酸镁治疗新生儿持续性肺动脉高压的临床效果[J].中外医疗,2016,35(12):46-47.
[6]张蓉,裘毅刚,邢娜,等.西地那非对慢性心力衰竭患者治疗效果及安全性的Meta分析[J].中国心血管病研究,2017,15(4):370-376.
[7]张颖,杨京华,李杰.口服西地那非治疗肺动脉高压1年疗效观察[J].心肺血管病杂志,2015,34(5):371-375.
[8]唐晓艳,王丹华.咖啡因在新生儿中的应用进展[J].中华新生儿科杂志,2014,29(5):343-346.
[9]李青,孙根义.西地那非的应用与对心血管疾病的影响[J].中国新药与临床杂志,2002,21(7):433-436.
[10]骆晓琴,袁伟,张学渊.枸橼酸西地那非导致听力损伤的研究进展[J].中华耳科学杂志,2012(4):533-535.
[11]潘晓靓,刘冬琳,孟巍,等.咖啡因暴露对小鼠胚胎发育的影响[J].武汉大学学报(医学版),2008,29(2):165-168.
[12]曲晓宇,董雷,张四喜,等.HPLC-MS/MS法同时检测抗疲劳药物及保健品中非法添加的7种壮阳类化学药物[J].中国药房,2013(33):3 129-3 131.
[13]蒋丽萍,屠婕红,徐宏祥,等.UPLC-MS/MS法测定抗疲劳类保健食品中非法添加的9种壮阳类化学药物[J].中草药,2015,46(15):2 238-2 245.
[14]张翠英,李振国,徐金铃,等.UPLC/MS/MS法检测补肾壮阳类中成药中非法添加枸橼酸西地那非的定性定量研究[J].中国卫生检验杂志,2007,17(10):1 741-17 42.
[15]邹冬梅,袁宏球,吴琼,等.咖啡及其制品中咖啡因HPLC测定的前处理方法研究[J].热带作物学报,2014,35(1):176-182.
[16]王胜,谭慧,朱其明.GB 5009.139-2014饮料中咖啡因测定色谱条件的探讨[J].公共卫生与预防医学,2016,27(2):119-121.
[17]GB/T 5009.197-2003保健食品中盐酸硫胺素、盐酸吡哆醇、烟酸、烟酰胺和咖啡因的测定[S].
[18]SN/T 4054-2014出口保健食品中育亨宾、伐地那非、西地那非、他达那非的测定液相色谱-质谱质谱法[S].
[19]陈军.HPLC法同时测定黄酒中4种非法食品添加剂[J].化学分析计量,2014,23(3):61-63.
[20]马莹,周胜菊.UPLC-DAD法测定凤冈锌硒茶酒中的咖啡因[J].中国茶叶,2016(7):14-15.
[2]魏博通,陈力.我国保健酒市场发展的现状存在的问题与对策分析[J].商场现代化,2010(35):64-65.
[3]李安陵.关于保健酒的研发思考[J].酿酒,2009,36(5):87-90.
[4]陈玲,张炼,李文斌.不同剂量西地那非治疗新生儿肺动脉高压的疗效[J].华中科技大学学报(医学版),2012,41(2):210-213.
[5]王岩.西地那非联合硫酸镁治疗新生儿持续性肺动脉高压的临床效果[J].中外医疗,2016,35(12):46-47.
[6]张蓉,裘毅刚,邢娜,等.西地那非对慢性心力衰竭患者治疗效果及安全性的Meta分析[J].中国心血管病研究,2017,15(4):370-376.
[7]张颖,杨京华,李杰.口服西地那非治疗肺动脉高压1年疗效观察[J].心肺血管病杂志,2015,34(5):371-375.
[8]唐晓艳,王丹华.咖啡因在新生儿中的应用进展[J].中华新生儿科杂志,2014,29(5):343-346.
[9]李青,孙根义.西地那非的应用与对心血管疾病的影响[J].中国新药与临床杂志,2002,21(7):433-436.
[10]骆晓琴,袁伟,张学渊.枸橼酸西地那非导致听力损伤的研究进展[J].中华耳科学杂志,2012(4):533-535.
[11]潘晓靓,刘冬琳,孟巍,等.咖啡因暴露对小鼠胚胎发育的影响[J].武汉大学学报(医学版),2008,29(2):165-168.
[12]曲晓宇,董雷,张四喜,等.HPLC-MS/MS法同时检测抗疲劳药物及保健品中非法添加的7种壮阳类化学药物[J].中国药房,2013(33):3 129-3 131.
[13]蒋丽萍,屠婕红,徐宏祥,等.UPLC-MS/MS法测定抗疲劳类保健食品中非法添加的9种壮阳类化学药物[J].中草药,2015,46(15):2 238-2 245.
[14]张翠英,李振国,徐金铃,等.UPLC/MS/MS法检测补肾壮阳类中成药中非法添加枸橼酸西地那非的定性定量研究[J].中国卫生检验杂志,2007,17(10):1 741-17 42.
[15]邹冬梅,袁宏球,吴琼,等.咖啡及其制品中咖啡因HPLC测定的前处理方法研究[J].热带作物学报,2014,35(1):176-182.
[16]王胜,谭慧,朱其明.GB 5009.139-2014饮料中咖啡因测定色谱条件的探讨[J].公共卫生与预防医学,2016,27(2):119-121.
[17]GB/T 5009.197-2003保健食品中盐酸硫胺素、盐酸吡哆醇、烟酸、烟酰胺和咖啡因的测定[S].
[18]SN/T 4054-2014出口保健食品中育亨宾、伐地那非、西地那非、他达那非的测定液相色谱-质谱质谱法[S].
[19]陈军.HPLC法同时测定黄酒中4种非法食品添加剂[J].化学分析计量,2014,23(3):61-63.
[20]马莹,周胜菊.UPLC-DAD法测定凤冈锌硒茶酒中的咖啡因[J].中国茶叶,2016(7):14-15.