生活污水中苯二氮䓬类药物及其新型策划药分析方法优化及应用
Optimization and Application of an Analytical Method for Benzodiazepines and Designer Benzodiazepines in Domestic Wastewater
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摘要: 近年来苯二氮䓬类药物及其新型策划药在全球范围内的滥用呈现上升趋势. 为实时监测区域苯二氮䓬类药物及其新型策划药的使用情况,该研究建立了利用固相萃取-高效液相色谱串联质谱(SPE-UPLC-MS/MS)技术检测污水中苯二氮䓬类药物及其代谢产物的分析方法,并对前处理条件和仪器参数进行了优化,前处理优化过程具体包括固相萃取柱类型、淋洗条件、洗脱条件及复溶条件的选择. 最后应用优化后的方法测定北京市6家污水处理厂实际进水样品. 结果表明:j前处理选用Cleanert PCX萃取柱,依次使用2 mL 2%(V/V)甲酸水溶液、2 mL甲醇淋洗填料,使用4 mL 5%(V/V)甲醇氨溶液洗脱目标化合物,氮吹后用500 μL 50%(V/V)甲醇水溶液复溶残留物时效果最优. k25种目标化合物不同浓度梯度加标回收率为85.7%~115%,基质效应、检出限和定量限、标准曲线及线性范围、精密度等指标均满足方法验证要求. l实际污水进水样品25种目标化合物可检出18种,浓度在0.03~22.4 ng/L,验证了方法的可靠性. 研究显示,该分析方法可用于检测生活污水中苯二氮䓬类药物及其新型策划药,可为进一步开展该类药物的污水流行病学研究提供参考依据.
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关键词:
- 苯二氮䓬类药物 /
- 代谢产物 /
- 污水流行病学 /
- 固相萃取-高效液相色谱-串联质谱联用仪
Abstract: The global prevalence of abuse of benzodiazepines (BZDs) and designer benzodiazepines (DBZDs) has witnessed a significant increase in recent years. To effectively monitor and control the presence of benzodiazepines in a specific region, a method combining solid phase extraction (SPE), ultra-performance liquid chromatography (UPLC), and triple quadrupole mass spectrometry (MS/MS) was developed. The optimization process involved the pretreatment process and UPLC-MS/MS parameter adjustments. The pretreatment optimization encompassed the selection of appropriate SPE column types, flushing and elution conditions, as well as resolution conditions. Subsequently, this method was applied to analyze the influent samples from six wastewater treatment plants in Beijing. The results showed that: (1) The most favorable outcomes were achieved using the Cleanert PCX extraction column, along with 2 mL of 2% (V/V) formic acid aqueous solution, 2 mL of methanol for flushing, 4 mL of 5% (V/V) methanol ammonia solution for elution, and 500 μL of a 50% (V/V) methanol-water solution for residue redissolution after evaporation. (2) By employing these optimized conditions, the recovery rates of 25 target compounds spanning various concentration ranges, were found to be between 85.7% to 115%, matrix effect, limits of detection and quantification, linear relationship, precision, and other performance indicators all met validation criteria. (3) The real influent samples revealed the detection and quantification of 18 out of the 25 target compounds, with concentrations ranging from 0.03 to 22.4 ng/L. The results indicated that the developed method enabled the detection of both BZDs and DBZDs in wastewater samples, which can serve as a valuable tool for further investigations on BZDs and DBZDs using wastewater-based epidemiology.
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