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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ZORBAX SB-C18(2.1 mm×150 mm,1.8μm)色谱柱,流动相为乙腈-0.1%磷酸溶液,梯度洗脱,流速为0.4 mL/min。采集210 nm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15 min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0.6~2 ng。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。
To establish an ultra-high performance liquid chromatography-diode-array (UPLC-DAD) detection method for rapid determination of 18 kinds of psychotropic drugs, such as barbiturate and chlordiazepoxide, for improving sleep health food. The sample was extracted by chloroform and concentrated, then the methanol was dissolved. The mobile phase consisted of acetonitrile-0.1% phosphoric acid solution with gradient elution at a flow rate of 0.4 mL / min on a ZORBAX SB-C18 (2.1 mm × 150 mm, 1.8 μm) column. A 210 nm chromatogram was collected for primary screening and quantification. Spectral libraries were constructed based on spectral characteristics of 18 drugs to confirm the identity of the compounds. The results showed that 18 kinds of psychotropic drugs could be effectively separated within 15 min. The correlation coefficients (r) were all greater than 0.999 in the linear range of 3 ~ 100 μg / mL, and the average recoveries were between 80.2% and 107.2%. The relative standard deviations Less than 7%, the detection limit of 0.6 ~ 2 ng. The method is simple, fast, sensitive and reproducible. Suitable for rapid screening of illicitly added chemicals in sleep-health supplements.