土壤及沉积物中25种芳香胺的固-液-液萃取及气相色谱-质谱测定方法初步研究

建立了土壤及沉积物中25种芳香胺的固-液-液萃取及气相色谱-质谱（GC-MS）测定方法。样品中的25种芳香胺在碱性条件下用水-甲基叔丁基醚共同萃取,并考察了碱液浓度对萃取效率的影响。结果表明,优化条件下方法的精密度（RSD）小于18%（n=6）,25种芳香胺的回收率有16种在50%以上,方法检出限（LOD,3σ）为0.11~1.90μg/kg。

A highly sensitive SPE-liquid/liquid extraction-RPLC analytical method for the determination of 6β-hydroxycortisol and cortisol in cancer patients' urine

A highly sensitive SPE-liquid/liquid extraction RPLC method has been developed for the analysis of 6β-hydroxycortisol and cortisol in the urine of cancer patients. Methods： After SPE column purification and liquid-liquid extraction, the sample test solutions were analyzed with RPLC using a C18 analytical column. This improved analytical method has been validated for linearity, accuracy （recovery from urine）, repeatability （within-day and between-day precision）, specificity, sensitivity, and stability. This SPE-liquid/liquid extraction-RPLC is rapid, simple, accurate and reproducible. The technique is particularly useful for monitoring the CYP3A activity of cancer patients in clinical settings. The results are expressed as the ratio of 6β-hydroxycortisol to cortisol. Results： The CYP3A activity from a total of 153 samples was measured using this improved method. Considerable variation in the CYP3A activity of different cancer patients has been documented. Thus, personalized medical treatment based on the individual metabolic enzyme activity level is necessary. Conclusion： This new analytical method facilitates such individualized medical treatments.

SPE-HPLC-ELSD法测定复方藏药制剂肝纤消颗粒中黄芪甲苷的含量

目的:建立SPE-HPLC-ELSD法测定复方藏药制剂肝纤消颗粒中黄芪甲苷含量的方法。方法:采用固相萃取系统对肝纤消颗粒进行处理,色谱柱为Alltima C18(4.6 mm×250 mm,5μm),流动相乙腈-水(33∶67),流速1.0 mL.min-1,柱温35℃,ELSD漂移管温度110℃,载气流量2.7 L.min-1,进样量20μL。结果:黄芪甲苷在1.014～20.280μg峰面积积分值自然对数与进样量自然对数有良好的线性关系线,r=0.999 3;平均加样回收率为100.1%,RSD 2.6%。结论:该方法操作简单,准确,重复性好,可用于藏药肝纤消颗粒的质量控制。