Abstract

An adsorbent for HPLC, silica doubly layer-by-layer modified with 6,10-ionene and dextran sulfate, is obtained. The adsorbent has both hydrophobic and hydrophilic and ion-exchange properties (because of the presence of hydrophobic anions and cations on the surface). A possibility of using the obtained adsorbent in HPLC with tandem mass spectrometric detection is shown. The conditions for the separation of caffeine, paracetamol, doxylamine, and chlorpheniramine in the isocratic mode are selected in elution with mixtures of acetonitrile and an acetate buffer solution. The most successful results are achieved by eluting the separated substances with the mobile phase acetonitrile–15 mM acetate buffer solution (glacial acetic acid/ammonium acetate with pH 5.55 in the ratio 10 : 90, vol). Gradient elution conditions are selected, a methodology is developed for determining traces of pharmaceuticals in human serum in the multiple reaction monitoring (MRM) mode using the internal standard method. The source and MRM transition parameters are selected individually for each compound. The linear range of the calibration curve for paracetamol and caffeine is 0.5–200 ng/mL and for doxylamine and chlorpheniramine, 0.05–50 ng/mL. The concentration of pharmacologically active compounds of caffeine, paracetamol, doxylamine, and chlorpheniramine in the blood serum of patients taking appropriate drugs is 165.2, 17.3, 10.2, and 35.3 ng/mL, respectively.

中文翻译：

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高效液相色谱-串联质谱法测定6,10-氧化烯和硫酸右旋糖酐双重修饰的二氧化硅上的药理活性含氮化合物

摘要

获得了用于HPLC的吸附剂，用6,10-紫罗兰和硫酸右旋糖酐进行双层层层修饰的二氧化硅。吸附剂既具有疏水性又具有亲水性和离子交换特性（由于表面上存在疏水性阴离子和阳离子）。显示了在串联质谱检测中将获得的吸附剂用于HPLC的可能性。在等度模式下分离咖啡因，对乙酰氨基酚，多西拉敏和扑尔敏的条件是在用乙腈和乙酸盐缓冲溶液的混合物洗脱时选择的。用流动相乙腈– 15 mM乙酸盐缓冲溶液（冰乙酸/乙酸铵，pH 5.55，体积比为10：90）洗脱分离的物质可获得最成功的结果。选择梯度洗脱条件，开发了一种使用内标方法以多反应监测（MRM）模式确定人血清中药物痕量的方法。为每种化合物分别选择源和MRM过渡参数。对乙酰氨基酚和咖啡因的校准曲线的线性范围为0.5–200 ng / mL，而多西拉敏和扑尔敏的校准曲线的线性范围为0.05–50 ng / mL。服用适当药物的患者血清中咖啡因，对乙酰氨基酚，多西拉敏和扑尔敏的药理活性化合物浓度分别为165.2、17.3、10.2和35.3 ng / mL。对乙酰氨基酚和咖啡因的校准曲线的线性范围为0.5–200 ng / mL，而多西拉敏和扑尔敏的校准曲线的线性范围为0.05–50 ng / mL。服用适当药物的患者血清中咖啡因，对乙酰氨基酚，多西拉敏和扑尔敏的药理活性化合物浓度分别为165.2、17.3、10.2和35.3 ng / mL。扑热息痛和咖啡因的校准曲线的线性范围是0.5–200 ng / mL，而多西拉敏和扑尔敏的校准曲线的线性范围是0.05–50 ng / mL。服用适当药物的患者血清中咖啡因，对乙酰氨基酚，多西拉敏和扑尔敏的药理活性化合物浓度分别为165.2、17.3、10.2和35.3 ng / mL。