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混合型离子交换反相吸附固相萃取柱串联萃取-超高效液相色谱-串联质谱法测定地表水中32种抗生素的含量 被引量:8
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作者 张蓓蓓 孙慧婧 吉鑫 《理化检验(化学分册)》 CAS CSCD 北大核心 2022年第8期893-901,共9页
500 mL地表水样经0.45μm滤膜过滤后,加入0.4 g乙二胺四乙酸二钠,以约2 mL·min^(-1)上样速率过已串联好的由混合型阳(MCX小柱)、阴(MAX小柱)离子交换反相吸附固相萃取柱。上样完毕后,将2根小柱分开。MCX小柱先用2%(体积分数,下同)... 500 mL地表水样经0.45μm滤膜过滤后,加入0.4 g乙二胺四乙酸二钠,以约2 mL·min^(-1)上样速率过已串联好的由混合型阳(MCX小柱)、阴(MAX小柱)离子交换反相吸附固相萃取柱。上样完毕后,将2根小柱分开。MCX小柱先用2%(体积分数,下同)甲酸溶液10 mL淋洗,再用氮气吹扫30 min,然后依次用甲醇4 mL、含5%(体积分数,下同)氨水的甲醇溶液4 mL洗脱。MAX小柱先用5%氨水溶液10 mL淋洗,再用氮气吹扫30 min,然后依次用甲醇4 mL、含2%甲酸的甲醇溶液4 mL洗脱。合并两个小柱的洗脱液,用氮气浓缩至尽干,用50%(体积分数)乙腈溶液稀释至1.0 mL,加入各内标物,使其在上述溶液中的质量浓度达到20.0μg·L^(-1),混匀后过0.22μm滤膜,滤液进入超高效液相色谱仪,在BEH C色谱柱上以不同体积比的0.1%(体积分数)甲酸溶液-乙腈混合溶液进行梯度洗脱,分离后的四环素类、磺胺类、大环内酯类、喹诺酮类、β-内酰胺类、林可酰胺类等6类抗生素以串联质谱仪的电喷雾离子源正离子模式电离,多反应监测模式检测,内标法定量。结果显示:32种抗生素标准曲线的线性范围为1.0~50.0μg·L^(-1),检出限(3s)为0.3~1.4 ng·L^(-1);对实际地表水样品进行3个浓度水平的加标回收试验,回收率为48.5%~93.4%,测定值的相对标准偏差(n=6)为1.3%~17%。方法用于太湖流域8个水源地地表水的分析,检出了磺胺甲恶唑、磺胺间甲氧嘧啶、林可霉素、克林霉素、克拉霉素和诺氟沙星,最大检出量为33.9 ng·L^(-1)(林可霉素)。 展开更多
关键词 萃取柱串联 超高效液色谱-串联质谱法 抗生素 地表水
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固相萃取-高效液相色谱法测定葡萄酒多酚物质 被引量:4
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作者 翁鸿珍 岳泰新 成宇峰 《中国酿造》 CAS 北大核心 2009年第3期164-166,共3页
通过对固相萃取柱萃取条件选择优化,确定了利用高效液相色谱法测定葡萄酒中多酚物质时最佳样品预处理条件。结果表明,乙醚作为洗脱剂时,洗脱液体积为15mL,酒样pH值为葡萄酒自然pH值时,各多酚类物质分离效果最佳,提取率均较高。
关键词 固相萃取柱萃取 高效液色谱 多酚物质
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A highly sensitive SPE-liquid/liquid extraction-RPLC analytical method for the determination of 6β-hydroxycortisol and cortisol in cancer patients' urine 被引量:3
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作者 Zhang Hong Fang Yu Li Ying Liang Aibin 《Journal of Medical Colleges of PLA(China)》 CAS 2010年第2期75-83,共9页
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-l... 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. 展开更多
关键词 Solid phase extraction (SPE) Liquid/liquid extraction Reversed-phase high performance liquid chromatography (RPLC) CYP3A 6β-hydroxycortisol/cortisol Cancer
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