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

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 C_(18) MGⅢC_(18)色谱柱(150 mm×2.0 mm,5μm),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10μL,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。

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 MGⅢC18(150 mm×2.0 mm,5μm).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 10μL.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.