安神类保健品中违禁化学药物的HPLC-DAD法测定研究
|
摘要
目的建立安神类保健品中违禁化学药物的HPLC-DAD测定方法。方法色谱柱为Thermo C_(18)(250 mm×4.6 mm,5μm),流动相A为乙腈,流动相B为含0.1%乙酸的0.01 mol·L~(-1)乙酸铵水溶液,梯度洗脱,流速1.0 mL·min~(-1),柱温35℃,检测器DAD,检测波长220 nm,进样量10μL。结果青藤碱、佐匹克隆、褪黑素、文法拉辛、氯苯那敏、罗通定、扎来普隆线性范围依次为1.42～57.0μg·mL~(-1)(R~2=0.9996)、1.52～60.7μg·m L~(-1)(R~2=0.9995)、1.41～56.4μg·mL~(-1)(R~2=0.9999)、1.36～54.3μg·mL~(-1)(R~2=0.9998)、1.52～60.9μg·m L~(-1)(R~2=0.9999)、1.75～70.0μg·mL~(-1)(R~2=0.9996)、1.58～63.0μg·mL~(-1)(R~2=1.0000),加样回收率均大于91.0%,RSD均小于1.8%。结论本方法灵敏度、准确度高、重复性好,为安神类保健品的质量控制提供了更为科学快捷的方法。
Objective To establish an HPLC-DAD method to determine the prohibited chemicals in sleepimproving health-food. Methods Thermo C_(18)(250 mm×4.6 mm, 5 μm) was used. Mobile phase A was acetonitrile; mobile phase B was 0.01 mol·L~(-1) ammonium acetate aqueous solution containing 0.1% acetic acid. Gradient elution was performed at a flow rate of 1.0 mL·min~(-1). The column oven temperature was 35 ℃, DAD, the detection wavelength was 220 nm, and the injection volume 10 μL. Results Sinomenine, zopiclone, melatonin, venlafaxine, chlorpheniramine, lootidine, and zaleplon showed good linearity at 1.42-57.0 μg·mL~(-1)(R~2= 0.9996), 1.52-60.7 μg·mL~(-1)(R~2= 0.9995), 1.41-56.4 μg·mL~(-1)(R~2= 0.9999), 1.36-54.3 μg·mL~(-1)(R~2= 0.9998), 1.52-60.9 μg·m L~(-1)(R~2= 0.9999), 1.75-70.0 μg·mL~(-1)(R~2= 0.9996), and 1.58-63.0 μg·mL~(-1)(R~2= 1.0000). The recoveries were more than 91.0%, and RSD less than 1.8%. Conclusion The method has good sensitivity, accuracy and reproducibility, which can control the quality of sleep-improving health-food.
Objective To establish an HPLC-DAD method to determine the prohibited chemicals in sleepimproving health-food. Methods Thermo C_(18)(250 mm×4.6 mm, 5 μm) was used. Mobile phase A was acetonitrile; mobile phase B was 0.01 mol·L~(-1) ammonium acetate aqueous solution containing 0.1% acetic acid. Gradient elution was performed at a flow rate of 1.0 mL·min~(-1). The column oven temperature was 35 ℃, DAD, the detection wavelength was 220 nm, and the injection volume 10 μL. Results Sinomenine, zopiclone, melatonin, venlafaxine, chlorpheniramine, lootidine, and zaleplon showed good linearity at 1.42-57.0 μg·mL~(-1)(R~2= 0.9996), 1.52-60.7 μg·mL~(-1)(R~2= 0.9995), 1.41-56.4 μg·mL~(-1)(R~2= 0.9999), 1.36-54.3 μg·mL~(-1)(R~2= 0.9998), 1.52-60.9 μg·m L~(-1)(R~2= 0.9999), 1.75-70.0 μg·mL~(-1)(R~2= 0.9996), and 1.58-63.0 μg·mL~(-1)(R~2= 1.0000). The recoveries were more than 91.0%, and RSD less than 1.8%. Conclusion The method has good sensitivity, accuracy and reproducibility, which can control the quality of sleep-improving health-food.
引文
[1]林芳,王一欣,李涛,等.安神类保健食品中新型非法添加药物的检测研究[J].食品安全质量检测学报,2016,7(4):1631-1636.
[2]张圆,闵春艳,郝刚,等.保健食品中非法添加化学药物的检测方法[J].中国执业药师,2014,11(7):35-39.
[3]何琳,王凌.色谱技术在检测中成药和保健食品中非法添加化学物质的应用研究进展[J].安徽医药,2011,15(10):1306-1309.
[4]鲁艺,韩东岐,黎雪清,等.安神类和抗风湿类中成药和保健食品中非法添加化学成分的案例分析[J].中国药事,2015,29(8):775-781.
[5]张莉,董建杰,郭芳华.合理使用镇静催眠药以防产生药物依赖性[J].河北医学,2006,12(11):1201-1202.
[6]肖丽和,刘吉金,关潇滢,等.镇静安神类中成药及保健食品中非法添加化学成分的快速筛查方法研究[J].中国当代医药,2009,16(14):15-16.
[7]葛文超,汤慧,张萍,等.高效液相色谱法同时测定镇静安神类中成药及保健食品中非法添加5种西药成分[J].安徽医药,2010,14(9):1018-1020.
[8]王永姣,张亚锋,李荣,等.保健食品中非法添加降糖药物的测定方法研究[J].安徽医药,2016,20(12):2269-2272.
[9]姜素芳,姚瑶,丁燕飞,等.反相高效液相色谱法测定盐酸青藤碱纳米脂质体药物含量及包封率[J].中南药学,2005,3(4):213-215.
[10]杨丽君,ROCHHOLZ Gertrud.反相高效液相色谱法测定血清中的佐匹克隆[J].色谱,2002,20(3):256-258.
[11]兰文,李昌亮,黄海.高效液相色谱法测定复方锌布颗粒中马来酸氯苯那敏和布洛芬的含量与有关物质[J].中南药学,2015,13(9):970-973.
[12]杜宁,周艳丽.高效液相色谱法测定盐酸文拉法辛含量及有关物质[J].北方药学,2012,9(3):4-5.
[13]魏嘉陵,林畅伟,苏茜. RP-HPLC测定脉舒静片中罗通定、利血平的含量[J].中国药学杂志,2004,40(1):60-61.
[14]药品检验补充检验方法和检验项目批准件批准件编号:2012004[S].国家食品药品监督管理局,2012.
[15]药品检验补充检验方法和检验项目批准件批准件编号:2013002[S].国家食品药品监督管理局,2013.
[2]张圆,闵春艳,郝刚,等.保健食品中非法添加化学药物的检测方法[J].中国执业药师,2014,11(7):35-39.
[3]何琳,王凌.色谱技术在检测中成药和保健食品中非法添加化学物质的应用研究进展[J].安徽医药,2011,15(10):1306-1309.
[4]鲁艺,韩东岐,黎雪清,等.安神类和抗风湿类中成药和保健食品中非法添加化学成分的案例分析[J].中国药事,2015,29(8):775-781.
[5]张莉,董建杰,郭芳华.合理使用镇静催眠药以防产生药物依赖性[J].河北医学,2006,12(11):1201-1202.
[6]肖丽和,刘吉金,关潇滢,等.镇静安神类中成药及保健食品中非法添加化学成分的快速筛查方法研究[J].中国当代医药,2009,16(14):15-16.
[7]葛文超,汤慧,张萍,等.高效液相色谱法同时测定镇静安神类中成药及保健食品中非法添加5种西药成分[J].安徽医药,2010,14(9):1018-1020.
[8]王永姣,张亚锋,李荣,等.保健食品中非法添加降糖药物的测定方法研究[J].安徽医药,2016,20(12):2269-2272.
[9]姜素芳,姚瑶,丁燕飞,等.反相高效液相色谱法测定盐酸青藤碱纳米脂质体药物含量及包封率[J].中南药学,2005,3(4):213-215.
[10]杨丽君,ROCHHOLZ Gertrud.反相高效液相色谱法测定血清中的佐匹克隆[J].色谱,2002,20(3):256-258.
[11]兰文,李昌亮,黄海.高效液相色谱法测定复方锌布颗粒中马来酸氯苯那敏和布洛芬的含量与有关物质[J].中南药学,2015,13(9):970-973.
[12]杜宁,周艳丽.高效液相色谱法测定盐酸文拉法辛含量及有关物质[J].北方药学,2012,9(3):4-5.
[13]魏嘉陵,林畅伟,苏茜. RP-HPLC测定脉舒静片中罗通定、利血平的含量[J].中国药学杂志,2004,40(1):60-61.
[14]药品检验补充检验方法和检验项目批准件批准件编号:2012004[S].国家食品药品监督管理局,2012.
[15]药品检验补充检验方法和检验项目批准件批准件编号:2013002[S].国家食品药品监督管理局,2013.