Application of high performance liquid chromatography with diode array detector technology in the detection of illegally added chemical drugs in sleep aid dietary supplements
10.3760/cma.j.cn114015-20230607-00414
- VernacularTitle:高效液相色谱-二极管阵列检测器技术在助眠保健品非法添加化学药物检测中的应用
- Author:
Shuo XU
1
;
Wenfeng XU
1
;
Yongmei KUANG
1
;
Pengfei JIN
1
Author Information
1. 北京医院药学部/国家老年医学中心/中国医学科学院老年医学研究院/北京市药物临床风险与个体化应用评价重点实验室（北京医院），北京 100730
- Publication Type:Journal Article
- Keywords:
Chromatography, high pressure liquid;
Diode array detector technology;
Sleep initiation and maintenance disorders;
Dietary supplements;
Illicit drugs;
Hypn
- From:
Adverse Drug Reactions Journal
2024;26(2):93-100
- CountryChina
- Language:Chinese
-
Abstract:
Objective:To develop the method of high performance liquid chromatography with diode array detector (HPLC-DAD) technology for detection of 20 chemical drugs possibly added into sleep aid dietary supplements such as sulpiride, ethosuximide, lamotrigine, zolpidem tartrate, melatonine, burspirone hydrochloride, phenobarbital, midazolam maleate, haloperidol, carbamazepine, phenytoin sodium, oxazepam, nitrazepam, alprazolam, clonazepam, estazolam, fupentixol dihydrochloride, thiopental, thioridazine hydrochloride and diazepam.Methods:An Agilent Zorbax C 18 column (250 mm×4.6 mm, 5 μm) was used for the separation, with gradient elution of acetonitrile and ammonium dihydrogen phosphate aqueous solution (adjust pH to 3.0 with phosphoric acid) as the mobile phase at the flow rate of 0.8 ml/min. The column temperature was 25 ℃, and the detection wavelength was set at 220 and 280 nm. The specificity, system adaptability, linear relationship, limit of detection, limit of quantitation, recovery, precision, stability and repeatability of the HPLC-DAD technology in detection of the above 20 chemical drugs was evaluated. Results:The HPLC-DAD technology had good specificity in detection of 20 chemical drugs, and the drug concentration had good linear relationship with peak area within certain ranges (correlation coefficients r ≥0.999 8). The average recoveries of 9 injections of 20 chemical drugs at low, medium, and high concentrations were 98.68%-99.85%, and the relative standard deviations of peak area variation were 0.57%-1.16%. The precision, repeatability, and stability of the method in detecting 20 chemical drugs were good. The limits of detection and quantitation were 0.05-1.59 μg/ml and 0.16-5.09 μg/ml, respectively. The established method was used to test 6 samples, and nitrazepam was detected in 1 sample. Conclusions:The established method is accurate, easy to operate, and easy to promote. It can be used for the detection of 20 chemical drugs that may be added into sleep aid dietary supplements.
