高效液相色谱法测定岩舒注射液中苦参碱的含量

目的：建立岩舒注射液中苦参碱的反相高效液相色谱法。方法：采用C18柱，流动相为甲醇－水－氨水（195：60：2．25），检测波长为220nm。结果：苦参碱在0．052－1．04μg范围内线性关系良好（r=0.9985)，日内和日间精密度RSD均小于2．0％，方法的平均回收率为99．5％。结论：本法简便、快捷，结果准确。     

氟罗沙星原料药中的杂质检查

目的　采用反相高效液相色谱法进行氟罗沙星原料药的杂质限量检查。方法　以乙腈-三乙胺及磷酸混合液 (15∶85)为流动相 ,Phenomenex C₈柱 (2.50mm×4.6mm ,5 μm)为固定相 ,流速为1.0ml·min^-1,检测波长为 286nm。结果　通过自身对照法用面积归一化法计算的氟罗沙星原料药中杂质含量均未超过 1%。结论　方法简单、灵敏度高 ,可用于氟罗沙星原料药的杂质含量测定。     

氟罗沙星原料药中的杂质检查

目的　采用反相高效液相色谱法进行氟罗沙星原料药的杂质限量检查。方法　以乙腈 三乙胺及磷酸混合液 (15∶85 )为流动相 ,PhenomenexC8柱 (2. 5 0mm× 4 . 6mm ,5 μm)为固定相 ,流速为 1 .0ml·min 1,检测波长为 286nm。结果　通过自身对照法用面积归一化法计算的氟罗沙星原料药中杂质含量均未超过 1%。结论　方法简单、灵敏度高 ,可用于氟罗沙星原料药的杂质含量测定。     

Development of photo-amino acid derivative reactivity assay: a novel in chemico alternative method for predicting photoallergy

Photoallergy test of cosmetics and several types of pharmaceutical substances is often necessary for obtaining approval from authorities. However, there are no official test guidelines for photoallergy evaluation. Therefore, we tried to establish a photoallergy test by utilizing an in chemico alternative sensitization method, amino acid derivative reactivity assay (ADRA). To determine the criteria for judging the photoallergy potential, photo-ADRA with or without photoirradiation was performed using 60 photoallergenic chemicals, and cysteine and lysine derivatives were detected using high-performance liquid chromatography either by absorbance or fluorescence measurement. The accuracy of prediction was 81.4% (48 of 59) and 80.0% (48 of 60) using the absorbance and fluorescence methods, respectively. However, as chemicals can breakdown into multiple chemicals during photoirradiation, the absorbance method often cannot perform accurate detection due to co-elution, whereas the fluorescence method can do this due to lack of co-elution. Moreover, all eight chemicals that were found to be negative or false-positive for photoirritation in the 3T3 neutral red uptake phototoxicity test were confirmed as positive for photoallergy using this method. Furthermore, we prepared three types of pseudo-mixtures where we added one photoallergen along with five nonphotoallergens and performed the photo-ADRA by the ultraviolet and fluorescence methods. The result of the fluorescence method was almost the same as that obtained with the use of a single photoallergen and hence the outcome was not affected by the mixture. Thus, this study not only showed a method of evaluating the photoallergy potential of a single chemical but also a mixture, making it useful as an in chemico photoallergy alternative test.     

Investigation of antioxidant compounds in commercial pomegranate molasses products using matrix-solid phase dispersion extraction coupled with HPLC

Pomegranate is a well known fruit for its unique flavor, taste and health benefits. The medicinal properties of this fruits directly associated with the phenolic content present, with great anti-oxidant potential. The research is intended to develop matrix solid phase dispersion method (MSPD) and HPLC quantification of four major anti-oxidant marker constituents (vitamin C, gallic acid, rutin & ellagic acid) in pomegranate molasses samples. The effects of several important experimental parameters like type of dispersant, sample-dispersant ratio, solvents and its volume, time of extraction were investigated. A C₁₈ column with the specification (5?µm, 250?×?4.0?mm) was used for the separation. A gradient flow of mobile phase was selected after many trials containing 0.1%, v/v solution of orthophosphoric acid and acetonitrile. The flow rate was 1.0?mL/min; and the chromatograms were recorded at 254?nm. The validation parameters, like linearity (r²?=?0.9985, 0.9965, 0.9925 & 0.9986), accuracy (100.3, 99.5, 100.9 & 101.9%), intra-day precision (%RSD?=?1.09, 1.02, 1.26 & 0.97), inter-day precision (%RSD?=?1.32, 0.83, 1.07, & 1.15) LOD (0.07, 4.50, 0.45 & 0.40?µg/mL), LOQ (0.095, 9.50, 0.85 & 9.5?µg/mL) and robustness (% RSD?=?0.92, 0.76, 0.81 & 0.83) respectively for vitamin C, gallic acid, rutin & ellagic acid, were found satisfactory as per ICH guidelines.     

阿魏酸钠胶囊与片剂在健康人体的生物等效性研究

目的：研究阿魏酸钠胶囊和阿魏酸钠片在健康志愿受试者中的药动学和人体生物等效性。方法：20名健康志愿者随机交叉单次口服受试制剂阿魏酸钠胶囊和参比制剂阿魏酸钠片,均100 mg,采用HPLC-UV检测方法,测定血浆中阿魏酸钠浓度,采用Das2.1程序计算其药动学参数,评价两种制剂的人体生物等效性。结果：受试制剂及参比制剂主要药动学参数分别为：Cmax（1.021±0.286）μg/ml和（1.066±0.397）μg/ml,tmax（0.388±0.078）h和（0.371±0.083）h,t1/2（0.887±0.431）h和（0.824±0.404）h,AUC（0~t）（0.613±0.172）μg.h/ml和（0.614±0.235）μg.h/ml。结论：受试制剂阿魏酸钠胶囊和参比制剂阿魏酸钠片具有生物等效性。     

HPLC法测定藜芦生品和醋制品中藜芦胺碱(veratramine)的含量

目的:建立HPLC法测定藜芦(Veratrum nigrumL.)生品和醋制品中生物碱藜芦胺碱(veratramine)的含量。方法:利用HPLC-UV色谱法测定。色谱柱为Scienhome Kromasil C18柱,流动相为乙腈∶水∶三乙胺=52∶48∶0.03,流速为1 ml/min,柱温25℃,检测波长230 nm。结果:藜芦胺碱在0μg~40μg内与峰面积呈良好的线性关系,r=0.9995(n=7);藜芦生品中藜芦胺碱平均回收率为97.7%,RSD为2.39%。结论:本法简单可行,准确可靠,可以作为藜芦生品和醋制藜芦中生物碱藜芦胺碱(veratramine)含量测定方法。藜芦醋制后使藜芦胺碱(veratramine)溶出率高于生品。     

HPLC法测定人血浆中头孢羟氨苄含量

目的：建立用内标法测定人血浆中头孢羟氨苄浓度的HPLC方法。方法：用c（高氯酸）=10％直接沉淀血浆蛋白。以对氨基苯甲酸为内标，测定血浆中头孢羟氨苄的浓度。结果：血浆中杂质不干扰样品峰和内标峰，20．00、2．00、0．20μg／mL的回收率分别为98．10％、98．70％、91．10％；批内精密度高、中、低浓度分别为3．80％，5．60％，7．30％;批间精密度高、中、低浓度分别为4．10％，6．50％，9．70％，最低检测限为0．10μg／mL，线性范围为0．20～30．00μg／mL。结论：本法稳定、精密度好，准确可靠，适用于头孢羟氨苄血浆浓度测定。     

淫羊藿次苷Ⅰ在大鼠体内的药动学和组织分布研究

 目的研究淫羊藿次苷Ⅰ在血液和各组织中的HPLC检测方法及在大鼠体内的药动学和组织分布。方法采用Dikma-C₁₈色谱柱(4.6mm×250mm,5μm),流动相甲醇-0.2%磷酸(73:27),流速1.0mL·min^-1,检测波长270nm,柱温20℃。大鼠按淫羊藿次苷Ⅰ单剂量10mg·kg^-1尾静脉注射后,采用高效液相色谱法测定给药后不同时间的淫羊藿次苷Ⅰ血药浓度和各组织浓度,用3P97程序计算药动学参数。结果淫羊藿次苷Ⅰ的血药浓度-时间曲线符合二室模型,并在心脏和肌肉组织有一定程度的蓄积。结论此方法简便、准确、稳定,可用于淫羊藿次苷Ⅰ的药动学和组织分布研究。     

Variability and uncertainty assessment of patulin exposure for preschool children in Flanders.

The objective of the present study was to evaluate the patulin exposure of children consuming organic, handcrafted or conventional apple juice through a probabilistic approach and to evaluate the effectiveness of several risk management options aiming to reduce the risk for children due to patulin exposure. However, a large part of the data on patulin contamination of apple juice fell under the limit of detection (LOD). Different methods were tested to deal with these so-called left censored data and a uniform distribution with uncertain bounds was selected to handle this censorship. Variability and uncertainty assessment of patulin exposure showed that 0.9% [90% confidence interval (CI): 0.3-1.8%] of the children consuming only organic apple juice exceed the tolerable daily intake (TDI). For consumers of conventional and handcrafted apple juice this was respectively 0.1% [90% CI: 0-0.3%] and 0% [90% CI: 0-0.2%]. Reduction of the patulin contamination in apple juice to concentrations below 25 microg/kg reduced the percentage of the children exceeding the TDI to 0% [90%CI: 0-0.2%] for organic apple juice. Reduction of the apple juice consumption was less effective than a reduction of the patulin concentration in apple juice and is only useful when the patulin concentration of apple juice is below 25 microg/kg.