School of Public Health, North China University of Science and Technology, Tangshan 063210, China.
Hebei Province Key Laboratory of Occupational Health and Safety for Coal Industry, School of Public Health, North China University of Science and Technology, Caofeidian, Tangshan 063210, China.
Molecules. 2021 Aug 27;26(17):5209. doi: 10.3390/molecules26175209.
A novel diatomite-supported zeolitic imidazolate framework-8 sorbent (ZIF-8@Dt-COOH) was in situ fabricated and developed for solid-phase extraction of three benzodiazepines (triazolam, midazolam and diazepam) in urine followed by high-performance liquid chromatography. ZIF-8@Dt-COOH was easily prepared by coating ZIF-8 on the surface of Dt-COOH and characterized by Fourier transform infrared spectra, X-ray powder diffractometry and scanning electron microscopy. Compared with bare Dt-COOH, the extraction efficiency of ZIF-8@Dt-COOH for the target was significantly increased from 20.1-39.0% to 100%. Main extraction parameters, including ionic strength and pH of solution, loading volume, washing solution, elution solvent and elution volume, were optimized in detail. Under optimum conditions, the developed method gave linearity of three BZDs in 2-500 ng/mL ( ≥ 0.9995). Limits of detection ( = 3), and limits of quantification ( = 10) were 0.3-0.4 ng/mL and 1.0-1.3 ng/mL, respectively. In addition, the average recoveries at three spiked levels (5, 10 and 20 ng/mL) varied from 80.0% to 98.7%, with the intra-day and inter-day precisions of 1.4-5.2% and 1.5-8.2%, respectively. The proposed method provided an effective purification performance and gave the enrichment factors of 24.0-29.6. The proposed method was successfully employed for the accurate and sensitive determination of benzodiazepines in urine.
一种新型的硅藻土负载沸石咪唑酯骨架-8 吸附剂（ZIF-8@Dt-COOH）被原位制备并发展用于尿液中三种苯并二氮杂䓬类药物（三唑仑、咪达唑仑和地西泮）的固相萃取，随后进行高效液相色谱分析。ZIF-8@Dt-COOH 是通过在 Dt-COOH 表面涂覆 ZIF-8 制备的，并用傅里叶变换红外光谱、X 射线粉末衍射和扫描电子显微镜进行了表征。与裸 Dt-COOH 相比，ZIF-8@Dt-COOH 对目标物的萃取效率从 20.1%至 39.0%显著提高到 100%。详细优化了主要萃取参数，包括溶液的离子强度和 pH 值、上样体积、洗涤液、洗脱溶剂和洗脱体积。在最佳条件下，该方法对三种 BZD 的线性范围为 2-500 ng/mL（≥0.9995）。检测限（S/N = 3）和定量限（S/N = 10）分别为 0.3-0.4 ng/mL 和 1.0-1.3 ng/mL。此外，三个加标水平（5、10 和 20 ng/mL）的平均回收率在 80.0%至 98.7%之间，日内和日间精密度分别为 1.4-5.2%和 1.5-8.2%。该方法提供了有效的净化性能，富集因子为 24.0-29.6。该方法成功用于尿液中苯并二氮杂䓬类药物的准确和灵敏测定。
