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1.
目的:建立测定甲氧氯普胺( MCP)鼻腔喷雾剂含量和有关物质的HPLC检测方法。方法采用Agilent TC-C18柱(250 mm ×4.6 mm,5μm),流动相为乙腈-磷酸盐缓冲液(取0.05 mol/L磷酸二氢钾溶液,加三乙胺5 ml,用磷酸调至pH 4.0)(19∶81),检测波长为275 nm,柱温30℃,流速为1.0 ml/min。结果与结论在建立的色谱条件下,MCP与有关物质峰基线分离,MCP浓度在10~200μg/ml 范围内线性关系良好,r=0.9999,回收率为100.3%~101.6%, RSD为0.68%(n=9),MCP检出限0.3 ng。该方法准确、可靠,重复性较好,可作为MCP鼻腔喷雾剂的质量控制方法。 相似文献
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HPLC法测定注射用阿奇霉素的有关物质 总被引:3,自引:0,他引:3
目的:建立注射用阿奇霉素有关物质的新检测方法。方法:采用高效液相色谱法(HPLC)检测注射用阿奇霉素中有关物质。液相色谱条件为色谱柱:Waters XBridgeTM Sheild RP18;流动相:乙腈-磷酸盐缓冲液(取0.05mol/L磷酸氢二钾溶液,用20%磷酸溶液调节pH值至8.6),流动相(58:42);流速:1ml·min^-1检测波长为210nm,柱温:30℃。结果:高效液相色谱法阿奇霉素的检测限为4.6ng,阿奇霉素主峰与杂质峰分离完全。结论:高效液相色谱法灵敏度高,可量化,更适用于注射用阿奇霉素的有关物质检查。 相似文献
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目的建立脑震宁颗粒中阿魏酸和橙皮苷含量的测定方法。方法采用高效液相色谱法,色谱柱为VP—ODSC18柱(250mm×4.6mm,5μm),流动相:甲醇-0.5%醋酸水(4:6),流速:1.OmL/min,柱温:25℃,检测波长:284nm。结果阿魏酸、橙皮苷的回归方程分别为Y=0.0052X+0.003,r=0.9995;Y=0.010IX+0.059,r=0.9995,其线性范围分别为0.027~0.405、0.050~0.750μg。结论本方法灵敏度高,重复性强,样品处理简便。可以作为脑镇宁颗粒的含量测定方法。 相似文献
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目的建立HPLC法测定乐脉胶囊中芍药苷和丹酚酸B的含量。方法芍药苷和丹酚酸B均采用C18(4.6mm×250mm,5μm)色谱柱;流动相分别为乙腈-0.05%磷酸(13:87)和乙腈-甲醇-1.7%甲酸溶液(4:27:69);检测波长分别为230和286nm,柱温为30℃,流速为1.0ml·min^-1。结果芍药苷在0.20403—4.0806μg范围内得芍药苷回归方程Y=1×10^6X+2631(r=0.9999);丹酚酸B在0.12573~2.5147μg范围内得回归方程Y=937308X+560947(r=0.9996),两组分分别与峰面积呈良好的线性关系。芍药苷的平均回收率为98.9%,RSD为1.8%;丹酚酸B平均回收率为100.4%,RSD为2.8%。结论该方法结果准确,重复性好,可作为乐脉胶囊质量控制的定量方法。 相似文献
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HPLC法测定复方银杏叶胶囊中总黄酮醇苷的含量 总被引:1,自引:0,他引:1
目的测定复方银杏叶胶囊中总黄酮醇苷的含量,为制剂质量控制提供依据。方法采用反相高效液相色谱法,色谱柱:Shiseido MG C18(5μm,4.6mm×250mm);流动相:甲醇-0.4%磷酸溶液(68:32);检测波长:378nm;外标法定量。结果各成分在一定浓度范围内线性良好,回归方程为:槲皮素Y=3.94945×10^-6X+8.992×10^-2,r=0.9999,线性范围为6~120μg·ml^-1;山奈素Y=8.34202×10^-6X+3.969×10^-2,r=0.9999,线性范围为3~60μg·ml^-1;异鼠李素Y=1.74581×10^-6X-6.13×10^-2,r=0.9999,线性范围为1~20μg·ml^-1。结论本法快速、准确,重复性好。 相似文献
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高效液相色谱法测定茜草双酯固体分散体中茜草双酯的含量 总被引:1,自引:0,他引:1
目的建立茜草双酯固体分散体中茜草双酯含量的测定方法。方法采用高效液相色谱法:色谱柱为Eurospher 100-5 C18色谱柱(250mm×4.6mm,5μm);流动相为甲醇-水(80:20);流速:1.0mL/min;检测波长:264nm。结果茜草双酯在20.0~100.0μg·mL^-1浓度范围内线性关系良好(r=0.9998),平均回收率为100.25%,RSD为1.13%。结论本方法专属性好,灵敏、可靠,适用于茜草双酯类制剂药物浓度的检测。 相似文献
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目的:应用高效液相色谱技术建立盐酸右哌甲酯缓释微丸有关物质检查和含量测定的方法。方法采用Agilent ZORBAX SB-C18色谱柱(250 mm ×4.6 mm,5μm);磷酸二氢钾溶液[25 mmol/L,三乙胺0.2%(v/v),磷酸调至pH 3.5]-甲醇(65∶35)为流动相,检测波长209 nm,流速1.0 ml/min,柱温40℃。结果在选定的色谱条件下,盐酸右哌甲酯与相关杂质分离良好,制剂辅料不干扰盐酸右哌甲酯的测定;检测限为81.12 ng/ml(S/N=3),在质量浓度2~30μg/ml范围内,盐酸右哌甲酯与峰面积线性关系良好,相关系数r为0.9995;平均回收率为100.83%,溶液在12 h内保持稳定( RSD为0.10%)。结论该方法简便、准确、专属性强,可用于盐酸右哌甲酯缓释微丸有关物质及其含量的测定。 相似文献
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HPLC法测定双黄连口服液中绿原酸和黄芩苷的含量 总被引:5,自引:1,他引:4
目的建立HPLC法同时测定双黄连口服液中绿原酸和黄芩苷含量的方法。方法色谱柱用十八烷基硅烷键合硅胶为填充剂(AgilentZORBAXEclipseXDB-C18,4.6mm×150mm,5Micron)。流动相A:甲醇-水-磷酸(50∶950∶5),流动相B:甲醇。梯度洗脱程序:0~30,A:95%~35%,B:5%~65%;流速:1ml/min,检测波长327nm。结果绿原酸和黄芩苷的保留时间分别约为10.6、24min,与各自相邻峰的分离度均〉1.5。以峰面积(X)对进样浓度(Y)线性回归,绿原酸回归方程:Y=0.03298X-0.09386,r=0.9999,线性范围5.040~45.36μg·ml^-1。黄芩苷回归方程:Y=0.05155X-1.2864,r=0.9999线性范围:44.88~403.9μg·ml^-1。绿原酸、黄芩苷回收率(n=6)分别为99.6%和100.0%、RSD分别为0.32%和1.0%。结论本方法与2005版中国药典法含量测定结果一致,准确度好且操作简便。 相似文献
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目的:建立盐酸左旋去甲基苯环壬酯( demethyl levophencynonate hydrochloride,L-LPC)片的含量及有关物质的分析方法。方法采用高效液相色谱法;色谱柱Capcel PAK C18柱, MGⅡ5μm,4.6 mm ×250 mm,Col:No.A4AD 02992(Shiseido,日本);流动相甲醇∶乙腈∶0.05 mol/L醋酸钠缓冲溶液(pH 5.0)为4∶3∶3;流速1.0 ml/min;检测波长220 nm;进样量20μl;柱温为室温。结果方法回收率为(100.15±0.73)%;溶液在8 h保持稳定(RSD为0.36%);在0.1~50μg/ml范围内线性关系良好,其回归方程为Y=81558X-4768.3(R2=1,n=3)。结论所建立的方法简便、准确、灵敏,专属性强,为该制剂含量测定、半成品测定及制剂稳定性研究提供了方法学依据。 相似文献
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目的建立HPLC法测定胸腺肽α1微乳中胸腺肽α1含量。方法色谱柱:Venusil XBP C18(4.6 mm×250 mm,5μm);流动相:流动相A:磷酸盐缓冲液(pH=5.7)-乙腈(92∶8),流动相B:乙腈;流速:1.0 ml.min-1;检测波长:210 nm;进样量:20μl。结果胸腺肽α1在0.01~0.1 mg.ml-1浓度范围内呈良好线性关系,线性方程Y=15 837 X+2.7636(r=1.0000),平均回收率为98.9%,RSD为0.12%(n=9)。结论该方法简单,结果可靠,可作为胸腺肽α1微乳中胸腺肽α1的含量测定方法。 相似文献
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One of the factors of the successful military career guidance Cadet schools students is preserving and promoting their health. Medical support of children and adolescents aged 10-17 years should include the full range of medical and preventive measures defined for this group. The state of providing outpatient care for pupils at the Cadet School in St. Petersburg was studied. These results show that full medical care in accordance with the standards can be based only on children's health clinics. It is important that the organization of medical support pupils cadet schools should be cooperate with civilian health care. 相似文献
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V. A. Serezhenkov I. A. Moroz G. A. Klevezal A. F. Vanin 《Applied radiation and isotopes》1996,47(11-12)
ESR-spectrometry was used to investigate radiation-induced paramagnetic centers in enamel of mammals: carnivores (polar bear and fox), ungulates (reindeer, European bison, moose), and man. Values at half the microwave power saturation of the radiation signal, P1/2, evaluated at room temperature, was found to range from 16 to 26 mW for animals and man. A new approach to discrimination of the radiation induced signal from the total ESR spectrum of reindeer enamel is proposed. ‘Dose-response’ dependencies of enamel of different species mammals were measured within the dose range from 0.48 up to 10.08 Gy. Estimations of ‘radiosensitivity’ enamel of carnivores and ungulates showed good agreement with radiosensitivity enamel of man by ESR method. 相似文献
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Analysis of the results of the international comparison of activity measurements of a solution of Fe
The results of an international comparison of activity measurements of a solution of 55Fe organized by the BIPM in 2005 are reported and analysed. This exercise, which follows the procedures of the CIPM mutual recognition arrangement to update older comparisons, is a renewal of the comparison organized by the BIPM that took place in 1978. A EUROMET comparison was organized in 1996 specifically to compare activity measurements of a 55Fe solution by means of liquid-scintillation techniques. Results of these three comparisons are presented and discussed in this paper.
The radionuclide solution was provided by the NPL, which also distributed the samples to the participants. The activity of the ampoules was measured by 16 laboratories using 12 methods producing 25 results. Some general considerations on uncertainty assessments pertaining to the different techniques used are drawn. The outcome of four different estimators is compared from which the presence of at least one outlier can be confirmed. Further measurements should be made to try to reduce the discrepancy between the results. To date the outcome of the present comparison does not show an improvement to that of the 1996 comparison. 相似文献
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D Gasparini 《La Radiologia medica》1987,73(4):304-309
A new method of non-surgical treatment of varicocele syndrome is described: it consists in sclerotherapy of spermatic vein by trans-femoral percutaneous catheterization with balloon-catheters. In 8 cases venous thrombosis has been induced by direct electric clotting. The techniques and a 6 months follow-up are discussed. It is pointed out that this procedure should be considered as the method of choice for tubular lesions and sub-fertility prophylaxis in young people and in childhood. 相似文献
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目的探讨延迟性脾破裂误漏诊原因和预防措施.方法回顾性分析总结12例延迟性脾破裂中的诊断和误漏诊的经验与教训.结果本组延迟性脾破裂的误漏诊5例(41.66%).对多发伤与脾破裂并存可能认识不足,外伤史轻微或伤员隐瞒外伤史,缺乏腹痛-缓解-突然再腹痛的典型病史,缺乏“对冲性脾破裂”力学分析和整体化诊断思路等为其误漏诊的主要原因.结论详细的外伤史和全面系统检查,重视腹以外多发伤掩盖腹内脏器伤及延迟性脾破裂可能.确立外伤-腹内脏器伤-脾破裂整体化诊断思路.不间断地辅以B超检查脾形态学变化和腹内有无积液,腹腔穿刺确定有无血腹、X线胸腹部检查观察左侧胸肋角和膈肌运动情况、必要时CT检查以尽早发现脾包膜下血肿,降低延迟性脾破裂误漏诊率. 相似文献