固相萃取-HPLC法同时测定盐酸帕洛诺司琼注射液中6种杂质

目的：固相萃取—高效液相色谱法同时测定盐酸帕洛诺司琼注射液中差向异构体、对映异构体、氮氧杂质等6种杂质的含量。方法：样品经1 mol·L-1氢氧化钠溶液调节pH,经Agilent Bond Elut C8固相萃取柱（200 mg,3 mL）去除大部分基质干扰,实现净化与富集,再用乙醇洗脱得到富集物。采用USP40盐酸帕洛诺司琼原料药已知杂质测定方法,以Astec CHIROBIOTIC?誖V（250 mm × 4.6 mm,5 μm）为色谱柱对其进行分离检测。结果：6种杂质在0.2~4.3 μg·mL-1范围内线性良好,相关系数r≥0.999 5,方法的检测限为0.056~0.065 μg·mL-1,低、中、高3个浓度的加样回收率为90.60%~105.7%。结论：本方法可用于同时检测盐酸帕洛诺司琼注射液中的6种杂质。     

Investigation of non-linear Mate1-mediated efflux of trimethoprim in the mouse kidney as the mechanism underlying drug-drug interactions between trimethoprim and organic cations in the kidney

The purpose of this study was to elucidate the involvement of Mate1 in the tubular secretion of trimethoprim and saturation of Mate1-mediated efflux to address the mechanisms underlying the pharmacokinetic drug interactions with trimethoprim. Trimethoprim is a more potent inhibitor of MATE2-K than MATE1 with K_i values (μM) of 0.030–0.28 and 2.4–5.9, respectively. Trimethoprim is a substrate of human MATE1 and MATE2-K with K_m values of 2.3 ± 0.9 and 0.018 ± 0.004 μM, and mouse Mate1, but not human OCT2, mouse Oct1 and Oct2. Pyrimethamine significantly reduced the renal clearance (CL_R) of trimethoprim (mL/min/kg) from 40.0 ± 5.1 to 20.1 ± 3.7 (p < 0.05). Trimethoprim was given to mice at three infusion rates (150, 500, and 1500 nmol/min/kg). Together with an increase in the plasma concentrations of trimethoprim, the CL_R (mL/min/kg) of trimethoprim decreased to 25.9 ± 3.2, 13.5 ± 5.7, and 8.92 ± 1.50 at the respective rates. Trimethoprim decreased the CL_R of rhodamine 123 in an infusion rate-dependent manner: 11.5 ± 1.3 (control), 5.17 ± 1.55, 1.31 ± 0.50, and 0.532 ± 0.180. These results suggest that Mate1 mediates the tubular secretion of trimethoprim, and at therapeutic doses, MATEs-mediated efflux can be saturated, and thereby, cause drug interactions with other MATE substrates.     

空气中苯系物及卤代烷烃化合物的毛细管气相色谱测定法

目的 探讨二硫化碳解吸-毛细管气相色谱法测定工作场所空气中苯系物及卤代烷烃的检测方法.方法 工作场所空气中的苯系物及卤代烷烃经活性炭管采集,二硫化碳解吸后,注入带氢火焰离子化检测器(FID)的气相色谱仪进行分析,以保留时间定性,峰面积定量.结果 苯、甲苯、对二甲苯、间二甲苯、邻二甲苯、乙苯、苯乙烯、四氯化碳、三氯甲烷、1,2-二氯乙烷的线性范围分别为0.019～81.600、0.018～91.200、0.018～88.800、0.018～56.800、0.011～92.000、0.012～63.200、0.018～93.200、0.449～2 298.400、0.252～1 287.000、0.076～390.000 mg/m3,回收率为88.4%～98.1%,RSD为1.0%～6.0%.结论 该方法能够有效分离和准确测定空气中苯系物及卤代烷烃化合物,具有较好的精密度与准确度,适合现场空气中该类化合物的测定.     

Amino Acid Content of Human Semen in Normal and Infertility Cases

Reports concerning the content of alpha-amino-nitrogen and amino-acids in human semen are few and results are different with authors. These variations could be explained by the no considerations of the changes due to liquefaction. In order to test this possible effect, measures were performed 30 mm, 1 h 30, 3 h and 5 h after seminal collection. Deproteinization was obtained with mixture of barium hydroxide and zinc sulfate. The data were compared to results of spermiogram. According to seminal parameters, 6 categories were distinguished. Measures showed a significant increase of the alpha-amino-nitrogen with time. The chromatography separation showed 19 different free amino-acids. The content of the most amino-acids increased with time except phosphoserine, taurine and ornithine; several amino-acids appear. In cases of azoospermia, levels of alpha-amino-nitrogen and amino-acids were lower. The content of amino-acids is not influenced by the spermatozoa count that seems to indicate their glandular origins. The free amino-acids content had to be considered in regard to cases with low liquefaction. But, in all cases it appears necessary to use a strictly standardized method since results are influenced with time.     

木鳖子提取液抗氧化活性的分析

 目的 用高效液相色谱法（high performance liquid chromatography,HPLC法）测定木鳖子提取液的抗氧化活性。方法 苯甲酸与Co²⁺催化过氧化氢产生的羟基自由基反应,生成多种羟基化物,HPLC法测定加入木鳖子提取液前后苯甲酸改变量,从而间接测定木鳖子提取液对羟基自由基的抗氧化活性。色谱柱：ODS-100 C18（5 μm,150 mm×4.6 mm）;流动相：甲醇-乙酸铵水溶液（0.02 mol/L,5：95）;检测波长：230 nm;柱温：25℃;流速：1.0 mL/min。结果 苯甲酸的线性范围为0.08~1.6 μg（r=0.999 7）,RSD<0.96%（n=6）。结论 木鳖子提取液有一定的抗氧化活性。     

反相高效液相色谱法测定盐酸美普他酚(2-氨基-6-甲基)-苯甲酸酯的含量

目的 建立反相高效液相色谱法(reversed phase-high performance liquid chromatography,RP-HPLC)测定盐酸美普他酚(2-氨基-6-甲基)-苯甲酸酯的含量。方法 采用C18(4.6 mm×150 mm,5 μm)色谱柱,0.02 mol/L醋酸铵水溶液(氨水调节pH...     

Concentration of antiepileptic drugs in persons with epilepsy: a comparative study in serum and saliva

Aim of the study: The monitoring of antiepileptic drugs (AEDs) in clinical setting is important for measuring the efficacy of drugs and their safety and in personalizing drug therapy. We investigated the levels of AED, carbamazepine (CBZ), phenytoin (PHT) and phenobarbital (PHB), to understand their association in saliva compared with those in serum during the therapy. Materials and methods: In this study, we performed a prospective study of 116 persons with epilepsy (PWE; mean age 26.90 ± 11.83 years). Serum and saliva samples were collected at trough levels from the patients, who were under the treatment of CBZ, PHT and PHB either alone or in combination of these drugs for at least three months. The drug levels were assessed by high-performance liquid chromatography. Results and conclusions: The number of males (n = 88; 75.86%) was higher than females (n = 28; 24.14%) among the recruited patients. The intake of CBZ, PHT and PHB was observed in 49.14%, 68.10% and 38.79% of PWE, respectively. The levels of these AEDs showed a significant correlation (p < 0.05) between serum and saliva. Interestingly, the levels of mono-therapy or bi-therapy showed a significant association (p < 0.05) between serum and saliva, however, there was no significant association in case of poly-therapy. This is the first report in the Indian population on simultaneous estimation of the three commonly used AEDs, such as CBZ, PHT and PHB in serum and saliva implicating their associations, either in mono-therapy or bi-therapy in PWE.     

反相气相色谱法测定溶剂在PBMA中的无限稀释活度系数

用反相气相色谱方法测定了１６种溶剂在聚甲基丙烯酸丁酯（ＰＢＭＡ）中３４３￣４３３Ｋ范围内的无限稀释活度系数,并用周浩等的高分子溶液分子热力学模型对实验结果进行了关联,结果令人满意。     

不同炮制方法对瑞香狼毒化学成分的影响

目的：考察不同炮制方法对瑞香狼毒化学成分的影响。方法采用系统预试法,包括理化和薄层色谱（TLC）鉴别,检测瑞香狼毒生品和炮制品中化学成分的异同。结果（1）瑞香狼毒生品和炮制品中均含有糖类、苷类、酚类、鞣质类、有机酸类、皂苷类、黄酮类、甾体、三萜类、香豆素内酯类成分,可能含有挥发油、油脂类成分。水提液中酚类、鞣质类和皂苷类成分有差异。（2）水提液中,奶制品的黄酮类成分含量较低;乙醇提取液中,生品和三种炮制品的黄酮类成分基本相同。（3）水提取液中,醋制品的香豆素内酯类成分含量较高;乙醇提取液中,奶制品的香豆素内酯类成分含量较低。（4）水提取液中,生品的萜类成分含量较高;乙醇提取液中,生品和奶制品的萜类成分含量较高。结论不同炮制方法对瑞香狼毒的化学成分都有影响。     

高效液相梯度洗脱法测定血清中氢化可的松和可的松的含量

目的　测定血清中氢化可的松和可的松的比值以反映人体肝脏 1 1 β -羟类固醇脱氢酶的活性 ,为其研究提供一个有效的分析手段。方法　HPLC -UV法 ,梯度洗脱 ,内标定量。结果　血清中氢化可的松在 50～ 2 0 0μg·L-1 、可的松在 1 0～ 50 μg·L-1 范围内其线性回归方程分别为Y =- 0 .42 5 +0 .0 1 0X、Y =- 0 .1 63 +0 .0 50X ,相对回收率分别为 (1 0 2 .5± 3 .6) %、(97.6± 6 .0 ) %。 82名健康志愿者血中氢化可的松和可的松的浓度分别为 (1 32 .2± 44 .5) μg·L-1 和 (1 9.7± 5 .0 ) μg·L-1 ,其比值为 6 .89± 2 .2 6。结论　本法操作简便、灵敏可靠 ,符合人体血样糖皮质激素测定的要求