高效液相质谱联用法测定改善睡眠类保健食品中的非法添加物

孙晓; 田仁芳; 董靖; 贾寒冰; 张亚锋

文章摘要

孙晓,田仁芳,董靖,等.高效液相质谱联用法测定改善睡眠类保健食品中的非法添加物[J].安徽医药,2019,23(6):1087-1090.

高效液相质谱联用法测定改善睡眠类保健食品中的非法添加物

Determination of illegally added chemical drugs in sleep-improving health-food by HPLC-MS

投稿时间：2017-12-27

DOI：

中文关键词: 改善睡眠类保健食品高效液相质谱联用法非法添加物

英文关键词: Sleep-improving health-food HPLC-MS Illegally added drug

基金项目:陕西省科学技术厅重点研发计划(2017SF-311)

作者	单位
孙晓	西安市食品药品检验所,陕西西安 710054
田仁芳	西安怡康医药连锁有限责任公司,陕西西安 710054
董靖	西安市食品药品检验所,陕西西安 710054
贾寒冰	西安市食品药品检验所,陕西西安 710054
张亚锋	西安市食品药品检验所,陕西西安 710054

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中文摘要:

目的建立安神类保健食品中非法添加物的高效液相质谱联用法(HPLC-MS)测定方法。方法采用CAPCELLPAK C₁₈ MG Ⅲ C₁₈色谱柱(150 mm×2.0 mm,5 μm),流动相为乙腈-0.01 mol/L乙酸铵溶液(含0.1%乙酸),梯度洗脱,流速0.3 mL/min,柱温35 ℃,进样量10 μL,采用质谱检测器,电喷雾正离子模式(ESI+),进行多反应监测(MRM)和扫描。结果青藤碱、佐匹克隆、褪黑素、文法拉辛、氯苯那敏、罗通定、扎来普隆分别在7.10~285(r=0.999 0)、7.60~304(r=0.999 5)、7.05~282(r=0.999 3)、6.80~272(r=0.998 9)、7.60~304(r=0.997 9)、8.75~350(r=0.998 3)、7.90~315(r=0.998 6) ng/mL范围内有良好的线性关系,加标回收率依次为97.2%(RSD=2.10%)、97.3%(RSD=1.06%)、96.0%(RSD=1.79%)、97.3%(RSD=1.63%)、99.1%(RSD=0.97%)、95.6%(RSD=0.79%)、98.5%(RSD=1.21%)。结论该方法灵敏度高、重复性好、准确度好,对常量、微量甚至痕量非法添加药物能做到准确测定。

英文摘要:

Objective To establish an HPLC-MS method for the determination of prohibited chemical drugs in sleep-improving health-food.Methods The column was CAPCELLPAK C18 MG Ⅲ C₁₈ (150 mm×2.0 mm,5 μm).The mobile phase was acetonitrile -0.01 mol/L ammonium acetate solution (containing 0.1% acetic acid).A gradient elution was used at a flow rate of 0.3 mL/min.The column temperature was set at 35 ℃,and the injection volume was 10 μL.Mass spectrometry detector and electrospray positive ion mode (ESI+) were adopted for multi reaction monitoring (MRM) and screening.Results Sinomenine,Zopiclone,Melatonin,Venlafaxine,Chlorpheniramine,Lootidine and Zaleplon showed good linearity in the ranges of 7.10-285 ng/mL (r=0.999 0),7.60-304 ng/mL (r=0.999 5),7.05-282 ng/mL (r=0.999 3),6.80-272 ng/mL (r=0.998 9),7.60-304 ng/mL (r=0.997 9),8.75-350 ng/mL (r=0.998 3),and 7.90-315 ng/mL (r=0.998 6),respectively.The average recoveries were 97.2%(RSD=2.10%),97.3%(RSD=1.06%),96.0%(RSD=1.79%),97.3%(RSD=1.63%),99.1%(RSD=0.97%),95.6%(RSD=0.79%) and 98.5%(RSD=1.21%),respectively.Conclusion The method has high sensitivity,good reproducibility and high accuracy,which achieves an accurate determination of the normal,minute or even trace amount of illegally added drugs.

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