摘要
建立同时快速测定改善睡眠类保健食品中违法添加巴比妥、氯氮卓等18种精神药物的超高效液相-二极管阵列（UPLC—DAD）检测方法。样品经氯仿超声提取，浓缩后甲醇转溶处理。采用ZORBAXSB—C18（2．1mm×150mm，1．8μm）色谱柱，流动相为乙腈-0．1％磷酸溶液，梯度洗脱，流速为0．4mL／min。采集210nm色谱图进行初筛和定量，并根据18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：18种精神药物在15min内可有效分离，在3-100μg／mL的线性范围内相关系数（r）均大于0．999，平均回收率在80．2％-107．2％之间，相对标准偏差均小于7％，检测限为0．6～2ng。该方法简便、快速、灵敏度高且重现性好。适用于改善睡眠类保健食品中非法添加化学药品的快速筛查。
A rapid method has been established for simultaneously determination of 18 psychoactive drugs, including Barbital, Clozapine, Chlordiazepoxide, Midazolam Maleate, Phenobarbital, Perphenazine, Promethazine Hydrochloride, Chlormezanone, Nitrazepam, Amobarbital, Oxazepam, Secobarbital Sodium, Estazolam, Lorazepam, Clomazepam, Alprazolam, Diazepam and Triazolam, by ultra performance liquid chromatography-photodiode array detector （UPLC-DAD）. The samples were extracted with chloroform solution by ultrasonic technique, condenced by water bath. and redissolved in methanol. Analyses were performed on ZORBAX SB-C18 column （2.1 mm×150 mm, 1.8 μm） with a mobile phase of acetonitrile -0.1% phosphoric acid changing by linear gradient elution, flow rate of 0.4 mL/min, detection wavelength of 210 nm for rapid screening and quantifying. Characteristic absorption spectral library of 18 psychoactive drugs have been established for identifying the compound. The results showed that the 18 psychoactive drugs can be effectively separated within 15min, and the standard curves had good linearity over the concentration range of 3-100 μg/mL with correlation coefficients （r） above 0.999. The average recoveries were from 80.2% to 107.2% with the relative stand deviations （RSDs） less than 7%. The detection limits of the 18 psychoactive drugs ranged from 0.6 ng to 2 ng. The method is simple and rapid with high sensitivity and good replicability, which is suitable for the rapid determination of the 18 psychoactive drugs illegally added in sleep improvement health food.
出处
《食品科技》
CAS
北大核心
2013年第9期303-308,共6页
Food Science and Technology
