反相/阳离子混合模式色谱柱测定氨甲环酸注射液中有关物质

目的:通过对新型填料色谱柱及流动相的筛选,建立高效液相色谱法检测氨甲环酸注射液中的有关物质,避免现行方法中离子对试剂的使用并降低盐的浓度。方法:采用Thermo Mixed-mode WCX色谱柱(150 mm×4.6 mm,5μm),以10 mmol·L^(-1)磷酸二氢钠溶液(用氢氧化钠溶液调pH至5.2±0.05)-水-乙腈(50∶5∶45)为流动相,等度洗脱,流速1.0 mL·min^(-1),柱温25℃,检测波长210 nm,进样量20μL。结果:氨甲环酸与4个已知杂质的色谱峰均能良好分离。氨甲环酸、杂质B、杂质C、杂质D和杂质E在一定浓度范围内与相应的峰面积呈良好的线性关系(r≥0.999);检测限分别为0.34、0.50、0.0056、0.0021、0.12μg·mL^(-1);4个已知杂质的平均加样回收率(n=9)分别为97.4%、100.5%、98.4%和96.6%,RSD分别为3.9%、0.24%、0.52%和1.4%;供试品溶液和对照品溶液在22 h内均稳定。5批样品中其他单杂检出个数及杂质总量均优于2020年版《中华人民共和国药典》方法。结论:本方法专属性强,灵敏度高,仅添加低浓度盐即实现氨甲环酸与4个已知杂质的良好分离,适用于氨甲环酸注射液中有关物质的测定。

Optimization of Sample Pretreatment for Determination of Polycyclic Aromatic Hydrocarbons in Estuarine Sediments by Gas Chromatography

This study examined levels of polycyclic aromatic hydrocarbons (PAHs) in estuarine sediments in Licun (Qingdao, China) by gas chromatography under optimized conditions for sample pretreatment via ultrasonic extraction, column chromatography, and thin layer chromatography. Methanol and dichloromethane (DCM)/methanol (2:1, v/v) were used in ultrasonic extraction, and DCM was used as eluate for column chromatography. The developing system consisted of n-hexane and DCM at a ratio of 9:1 (v/v), with DCM as the extraction solvent for PAHs-containing silica gel scraped off the plate. When the spiking level is 100 ng, total recoveries of spiked matrices for four target PAHs (phenanthrene, anthracene, pyrene and chrysene) were 83.7%, 76.4%, 85.8%, and 88.7%, respectively, with relative standard deviation (RSD) between 5.0% and 6.5% (n = 4). When the spiking level is 1000 ng, associated total recoveries were 78.6%, 72.7%, 82.7% and 85.3%, respectively, with RSD between 4.4% and 5.3% (n = 4). The opti-mized method was advantageous for determination of PAHs in complex matrix due to its effective sample purification.