HPLC同时测定苦参药材中苦参碱和氧化苦参碱的含量测定方法

目的探讨高效液相色谱法在测定苦参药材中苦参碱和氧化苦参碱的含量上的具体操作方法以及可行性。方法建立高效液相色谱法对中药苦参药材中的苦参碱和氧化苦参碱的含量进行测定,并且对该实验方法的精密度,重复性,稳定性等方面进行实验考察。结果得出样品苦参中含有苦参碱平均含量为0.083%,相对标准偏差—RSD是1.79%;氧化苦参碱平均含量为2.28%,相对标准偏差—RSD是1.65%。并且使用高效液相色谱对苦参中苦参碱和氧化苦参碱进行含量测定具有良好的精密度,重复性,稳定性,以及加样回收率。结论使用高效液相色谱法对苦参药材中的苦参碱和氧化苦参碱的含量进行实验测定,实验操作简单,方便,准确度高,稳定性好,同时重复性也比较理想,在对中药苦参中苦参碱和氧化苦参碱的含量测定方面具有良好的使用价值。     

注射用乳糖酸阿奇霉素含量测定

目的：比较微生物效价法与高效液相色谱法测定乳糖酸阿奇霉素含量的数据,以确定高效液相色谱法是否可以在工业生产中应用、推广。方法：建立高效液相色谱法测定乳糖酸阿奇霉素注射剂含量的方法学,分别按2000版药典的微生物法及新建立的高效液相色谱法对乳糖酸阿奇霉素粉针剂进行含量测定,用统计学方法比较两种方法测定的结果是否有统计学差异。结果：统计学分析结果表明两种方法测定乳糖酸阿奇霉素粉针剂的含量结果无统计学意义。结论：高效液相色谱法可以应用于乳糖酸阿奇霉素粉针剂的含量测定。     

高效液相色谱法测定白芍总苷中芍药苷含量

目的建立高效液相色谱对白芍总苷中芍药苷的含量进行检测的方法。方法利用高效液相色谱法对白芍总苷胶囊中的芍药苷的具体含量进行检测,并同时对高效液相色谱法对白芍总苷中芍药苷测定的精密度和重复性以及稳定性方面进行考察,分析可行性。结果白芍总苷样品中芍药苷的平均质量分数为368.12mg/g,相对标准偏差RSD是1.72%。芍药苷的回归方程为:Y=6.523 2X-0.821 69(r=0.999 9),线性范围是4.43～198.90μg/mL,并使用高效液相色谱法进行测定具有良好的精密度、重复性及稳定性。结论本研究建立的应用高效液相色谱法对白芍总苷中芍药苷的含量进行检测,其检测方法简单、方便、准确性好,同时实验稳定性和重复性也比较好,在对白芍总苷中芍药苷的含量测定上,具有良好的应用价值。     

高效液相色谱法测定头孢呋辛酯片含量的不确定度评定

目的：建立高效液相色谱法测定头孢呋辛酯片含量的不确定度评定方法。方法：通过对头孢呋辛酯片含量测定的检测过程中可能产生不确定度的来源进行分析,建立了该测定法的不确定度评定方法。结果：本批次头孢呋辛酯片供试品的高效液相色谱法含量测定结果为96.27%±1.16%（k=2）。结论：通过建立高效液相色谱法测定头孢呋辛酯片含量的不确定度评定方法,为该检测方法的不确定度计算提供了参考,同时也为检测过程中的误差控制提供了依据。     

HPLC测定甲硝唑片中甲硝唑的含量

目的 建立测定甲硝唑片中甲硝唑含量的高效液相色谱法。方法采用XDB柱,流动相为：甲醇-水（20∶80）的反高效液相色谱系统。结果甲硝唑在33.28～332.8 μg内呈良好的线性关系（r=0.999 9）,平均回收率为 99.8%。结论本方法简便,准确,重复性好,可用于甲硝唑片含量测定。     

高效液相色谱法测定芦荟中去氢木香内酯的含量

目的：建立高效液相色谱法测定芦荟中去氢木香内酯含量的体系。方法：采用高效液相色谱法,通过优化色谱条件（Hy-persilODS色谱柱,流动相为乙腈-水（70：30）,流速1.0mL·min-1,柱温30℃,检测波长为210nm,10uL进样）进行检测。结果：回归方程和相关系数为：A=1.68-3.34X104（r=0.9993）;线性范围为：0.023～0.182mg·ml-1,精密度试验RSD为0.895%,重复性试验RSD为1.52%,加样回收率为98.0%左右,平均含量为1.19mg/g。结果：高效液相色谱法测定芦荟中去氢木香内酯含量灵敏度高、专属性强、重现性好,可作为该制剂的质量控制方法。     

橘叶药材质量评价研究

目的建立橘叶药材的质量控制方法。方法对全国不同产地10批橘叶药材进行了生药学研究;采用高效液相色谱法建立了橘叶药材中橙皮苷的含量测定方法;对10批橘叶药材进行了水分、灰分、浸出物含量测定。结果选定的高效液相色谱法分离度好,回归方程来Y=2 857 969X-69 458,相关系数r=0.999 6;制定了水分、灰分、浸出物含量检测限。结论建立的质控方法简便易行、重复性好,测定结果真实可靠,可用于橘叶药材的质量评价。     

氢溴酸右美沙芬注射液含量测定及其降解物质检查

采用高效液相色谱法和紫外分光光度法测定氢溴酸右美沙芬注射液含量,并对高效液相色谱法和薄层色谱法检查注射液降解产物进行了比较。结果表明HPLC法既可准确测定注射液含量,又能准确检测出药物发生降解时药物定量变化。     

HPLC测定甲硝唑片中甲硝唑的含量

目的 建立测定甲硝唑片中甲硝唑含量的高效液相色谱法。方法采用XDB柱,流动相为：甲醇-水（20∶80）的反高效液相色谱系统。结果甲硝唑在33.28~332.8 μg内呈良好的线性关系（r=0.999 9）,平均回收率为 99.8%。结论本方法简便,准确,重复性好,可用于甲硝唑片含量测定。     

氨糖美辛肠溶片中吲哚美辛含量测定方法的比较研究

目的：比较氨糖美辛肠溶片中吲哚美辛3种含量测定方法的差异,对检测方法进行评价,选择一种最适宜的测定方法。方法：采用高效液相色谱法、紫外分光光度法及容量分析法对氨糖美辛肠溶片中吲哚美辛进行含量测定,对含量测定的结果、回收率、重复性以及各方法的优缺点进行比较和研究,并给出综合评价。结果：容量分析法作为现行标准的方法,回收率低,准确度差,质量控制水平低;高效液相色谱法测定结果准确,回收率高,重复性好;而紫外分光光度法操作简便,但重复性和专属性差于高效液相色谱法。结论：综合专属性、准确性等因素,高效液相色谱法优于其他两种方法,可用于氨糖美辛肠溶片的质量控制。     

尼麦角林残留量检验方法研究

目的通过对尼麦角林残留量高效液相色谱检验方法的验证,确定尼麦角林残留量用该检验方法检测的线性、灵敏度和回收率(准确度)。确保该方法对尼麦角林残留量浓度检测结果的准确性。方法高效液相色谱法。结果该检测方法的线性范围为1.0～15.0μg.mL-1;检测方法的回收率为99.4%,精密度与重复性良好;检测限为:0.001μg.mL-1;定量限为:0.009μg.mL-1。确定了凡残留量1.0～15.0μg.mL-1范围内,均可采用此方法检测。结论此方法操作简单,精密度、准确度、重复性较好。     

Isocratic RP-HPLC method for rutin determination in solid oral dosage forms

A rapid and sensitive assay for quantitative determination of rutin in oral dosage forms based on isocratic reversed phase high performance liquid chromatography (RP-HPLC) was developed and validated. Using a C(18) reverse-phase analytical column, the following conditions were chosen as optimal: mobile phase methanol-water 1:1 (v/v), pH 2.8 (adjusted with phosphoric acid), flow rate=1 mL min(-1) and temperature T=40.0 degrees C. Linearity was observed in the concentration range 8-120 microg mL(-1) with a correlation coefficient of 0.99982 and the limit of detection (LOD)=2.6 microg mL(-1), and limit of quantification (LOQ)=8.0 microg mL(-1). Intra- and inter-day precision were within acceptable limits. Robustness test indicated that the mobile phase composition and pH influence mainly the separation. The proposed method allowed direct determination of rutin in pharmaceutical dosage forms in the presence of excipients, but is not suitable for preparations where compounds structurally/chemically related to rutin may be present.     

Analysis of flavonoids from Cyclanthera pedata fruits by liquid chromatography/electrospray mass spectrometry

A liquid chromatography/mass spectrometry (LC/MS) based method was developed for the characterization of fruits of Cyclanthera pedata Scrabs (Caigua), a Peruvian food and medicinal plant. This method is based on the separation of flavonoid glycosides present in the methanolic extracts from C. pedata fruits using high performance liquid chromatography (HPLC) followed by detection with electrospray ionization mass spectrometry (ESI/MS). Chromatographic separation of the analytes of interest was achieved on a Symmetry C-18 column with detection in positive ion mode. Calibration graphs were obtained by determining the area ratio between external standard of each major compound and the internal standard naringine. Due to the sensitivity and the repeatability of the assay, this method is suitable for industrial quality control of raw materials and final products.     

Multicenter evaluation of a new inosine monophosphate dehydrogenase inhibition assay for quantification of total mycophenolic acid in plasma

The performance characteristics of a new inosine monophosphate dehydrogenase inhibition assay for the quantification of total mycophenolic acid (MPA) in plasma (Roche Diagnostics) were assessed in a multicenter evaluation. Validation data were collected from four institutions. Within-run and total imprecision were acceptable (n = 21 for each of 7 materials, coefficients of variation ranging 0.7-9.6%). The lower limit of quantification was 0.31 mg/L. The assay was linear from 0.31 to 15.0 mg/L. Method comparison with validated high-performance liquid chromatography with ultraviolet light or liquid chromatography tandem mass spectrometry methods showed good agreement (coefficients of correlation 0.974-0.994, slopes 1.01-1.17, intercepts -0.17 to 0.06). There was no difference found between results from different transplant types (cardiac vs. renal) or comedications (cyclosporine vs. tacrolimus). The recovery of samples from a proficiency testing scheme was acceptable. The cross-reactivity of AcMPAG, an in vitro active metabolite of MPA, was examined by adding AcMPAG to a pool of patient samples and subsequent quantification. MPA overestimation by AcMPAG cross-reactivity was found to be low (<5%). Thus, this interference is expected to be clinically irrelevant. In conclusion, the Roche Total MPA assay is a promising alternative for MPA quantification where chromatographic methods are not available.     

Automated determination of flutamide by a validated flow-injection method: application to dissolution studies of pharmaceutical tablets

The first flow-injection (FI) method for the determination of flutamide – a potent antiandrogen used for the treatment of prostate cancer – is reported. The method is based on the direct measurement of the absorbance of the analyte at 310 nm under flow conditions. Parameters affecting the determination such as detection wavelength, sample injection volume and flow rate were studied and optimized. The assay was validated (linearity, limits of detection and quantitation, accuracy, repeatability, reproducibility and selectivity) for the dissolution studies of flutamide-containing tablets during stability testing. The results were in good agreement with high performance liquid chromatography (HPLC) used as a reference method.     

Determination of isepamicin sulfate and related compounds by high performance liquid chromatography using evaporative light scattering detection

A simple reversed phase high performance liquid chromatographic method was developed for the analysis of isepamicin sulfate. The use of evaporative light scattering detection eliminates the need for sample derivatization. Separation of the isepamicin aminoglycoside from structurally similar related compounds was achieved using two Waters X-Terra RP18 columns connected in tandem at 10 degrees C. The assay of isepamicin sulfate and the estimation of its impurities was accomplished using external standard calibration curves at two sample concentrations: 1.6 mg ml(-1) for the analysis of isepamicin sulfate and 8.0 mg ml(-1) for the estimation of lower level impurities. The limit of detection was 0.1%. The specificity, assay linearity, low level assay linearity and assay repeatability were also investigated.     

Optimization and validation of a dissolution test for famotidine tablets using flow injection analysis

A dissolution test for famotidine tablets was optimized and validated using flow injection analysis (FIA). The effect of dissolution parameters such as pH, medium and stirring speed was studied, while the ruggedness of the procedure was validated. All measurements were performed using a simple direct spectrophotometric flow injection assay (lambdamax=265 nm) that has also been optimized and fully validated in terms of linearity, limit of detection, precision, selectivity and accuracy. Linearity was obeyed in the range 50-150% of famotidine (20-60 mg L-1), while the detection limit (0.1 mg L-1) and repeatability (sr<1.0%, n=12) were satisfactory. The sampling rate was 30 h-1. The dissolution results during quality and stability control of two batches of famotidine tablets obtained by the flow injection method were in good agreement with high-performance liquid chromatography (HPLC).     

丙泊酚中/长链脂肪乳注射液包封率分析方法的建立

目的：建立丙泊酚中/长链脂肪乳注射液包封率的分析方法。方法：利用超滤法分离微乳和游离药物,采用Agilent的XDB-C18作为色谱分离柱、乙腈-水（7∶3）为流动相、检测波长275 nm、柱温25℃、流速1.0 ml / min和进样量5μl进行色谱分析。结果：本方法重复性考察的RSD为1.14%。日间精密度考察RSD为1.25%。结论：所建立的包封率定量方法,简便、快速、重复性好,可作为工艺筛选过程中灵敏、高效、有区分力的监测方法。     

An automated method for the determination of subnanogram concentrations of eprinomectin in bovine plasma

Eprinomectin is a potent anthelmintic compound that kills certain parasitic nematodes and arthropods of cattle. A sensitive and automated bioanalytical assay was developed for quantitation of eprinomectin in bovine plasma in support of clinical development of eprinomectin for use in all classes of cattle. This assay determined the concentration of eprinomectin in plasma by reversed-phase high performance liquid chromatography (HPLC) with fluorometric detection. Plasma sample preparation included liquid extraction performed by the Packard MultiPROBE robotics workstation, followed by solid phase extraction performed by the Gilson ASPEC XL automated workstation. The HPLC assay included automated pre-column derivatization with a fluorogenic reagent system which included trifluoroacetic anhydride and N-methylimidazole as the catalyst. This reversed-phase chromatographic analysis was based on the fluorescence detection of derivatized eprinomectin and an internal standard, L-648 548, which was similarly derivatized by the fluorogenic reagents. The assay was automated and validated for two concentration ranges of 0.05–10 and 0.5–200 ng ml⁻¹. The lower limit of quantitation of eprinomectin in plasma was 0.05 ng ml⁻¹. The %RSD of the assay was 10% or better at all concentrations. This automated analysis of eprinomectin was used for high-throughput clinical assays with acceptable accuracy and precision.     

地塞米松片的溶出度

目的：研究并建立地塞米松片溶出度的介质及测定方法。方法：采用转篮法分别以1%盐酸，5%乙醇溶液，10%乙醇溶液，15%乙醇溶液及磷酸盐缓冲液（pH=6.6)5种溶出介质进行地塞米松片的溶出试验。以HPLC法测定溶出介质中地塞米松的浓度。结果：研制片与市售地塞米松片在5%乙醇溶液中45min时的溶出度均大于标示量的79%。结论 所建立的HPLC方法准确。可靠；地塞米松片在5%乙醇溶液中的溶出度符合药典要求。