建立超高效液相一二极管阵列检测方法,用于同时快速测定改善睡眠类保健食品中违法添加的14种精神药物(阿普唑仑、艾司唑仑、氯硝西泮、地西泮、马来酸咪达唑仑、三唑仑、硝西泮、巴比妥、氯氮卓、劳拉西泮、异戊巴比妥、奥沙西泮、苯巴比妥、司可巴比妥钠)。采用ZORBAXSB—C18(2.1mm×100mm,1.8μm)色谱柱,流动相甲醇.0.2%乙酸溶液,梯度洗脱,流速为0.4mL/min。采集210nm(0-7.70min)、230nm(7.70~13.50rain)色谱合成图进行初筛和定量。并根据14种药物的光谱特征建立光谱库,用于检出化合物的确证。结果表明:14种精神药物在13.5min内可有效分离,在5-50μg/mL或10~100gg/mL的线性范围内相关系数(n均大于0.9995,平均回收率在固体基质中为80.4%~106.2%;在液体基质中为80.7%~102.3%,相对标准偏差(RSD)都小于7%,检测限为3-6ng。该方法简便、快速、灵敏度高且重复性好。可作为检测改善睡眠类保健食品中违法添加化学药物的快速测定方法。
A method of ultra performance liquid chromatography-photodiode array detection (UPLC-DAD) has been established for the rapid simultaneous determination of 14 psychoactive drugs (alprazolam, estazolam, clonazepam, diazepam, phenobarbital, midazolam maleate, triazolam, nitrazepam, barbital, secobarbital, chlordiazepoxide, lorazepam, amobarbital, and oxazepam) that are illegally added in sleep-improving health-care foods. A ZORBAX SB-C18 column (2.1 mm × 100 mm, 1.8 μm) was applied. Methanol-0.2% acetic acid was selected as the mobile phase in a linear gradient elution mode,with flow rate of 0.4 mL/min. The detection wavelengths were 210 nm and 230 nm for rapid screening and quantitation. The results showed that the 14 psychoactive drugs could be effectively separated in 13.5 min, and the standard curves had good linearity over the concentration range of 5-50 μg/mL or 10-100 μg/mL. The correlation coefficients (r) were all above 0.9995. The average recoveries varied from 80.4%-106.2% and the detection limits were in the range of 3-6 ng for the psychoactive drugs. This developed method is characteristics of simple operation, rapid determirmdon, high sensitivity and excellent reproducib'dity so that it is suitable for the rapid determination of d 14 illegal psychoactive drugs in sleep-improving health-care foods.