测定山梨醇中镍含量的原子吸收分光光度法的建立与验证

目的 建立一种原子吸收分光光度法,定量检测山梨醇中的镍含量,并确认该方法的可行性.方法 采用标准加入法,在4份等量山梨醇样品中分别加入3 μg/ml镍标准母液0.0、0.5、1.0、1.5 ml.经10 g/L吡咯烷二硫代氨基甲酸铵溶液和甲基异丁基甲酮处理后,取萃取液,测定其在232.0 nm处的吸光度.结果 用标准加入法得到的标准曲线线性良好,决定系数＞0.998.镍加样回收率为98％～103％,测定结果的相对标准偏差为3％.该法测定镍的定量限为质量分数4.6×10-7.结论 建立的原子吸收分光光度法可以用于山梨醇中镍含量的定量检测.     

原子吸收分光光度法测定羧甲纤维素钠中的铅、铜含量

目的:建立原子吸收分光光度法测定羧甲纤维素钠中的铅、铜含量的分析方法.方法:样品经微波消解,采用石墨炉法测定铅含量,火焰法测定铜含量,并对测定方法进行了方法学考察.结果:方法线性关系良好,相关系数r>0.999,精密度试验RSD为1.6％～3.0％,平均回收率为90.1％～92.1％.结论:该方法准确,稳定且无干扰,可较好地用于羧甲纤维素钠铅、铜的含量测定.     

采用原子吸收分光光度法测定药用辅料硬脂富马酸钠中的重金属铅含量

目的建立石墨炉-原子吸收分光光度法测定硬脂富马酸钠中铅含量。方法硬脂富马酸钠经微波消解,赶酸后,按照拟定的仪器工作条件,采用石墨炉-原子吸收分光光度法测定硬脂富马酸钠中铅含量。结果铅元素在0~100μg·L~(-1)内与峰面积呈良好的线性关系(r=0.9999);高、中、低3个浓度平均回收率分别为96.8%、103.4%、92.1%,RSD分别为6.2%、1.3%、4.4%,说明本法准确度较好。结论本方法准确度高、重现性好,可用于硬脂富马酸钠中铅的含量测定,为建立药用辅料硬脂富马酸钠的质量标准提供参考。     

微波消解石墨炉原子吸收法测定葛粉中的铅

目的：建立葛粉中铅含量的测定方法。方法：采用微波消解法处理葛粉样品,加入20.0g/L磷酸二氢铵作为基体改进剂,用石墨炉原子吸收分光光度法测定铅含量。结果：加标回收率为95.23%～101.10%,RSD=4.68（n=6）,检出限为10μg/kg。结论：该法简单、快速、准确,可用于葛粉中铅的测定。     

原子吸收分光光度法测定复方锌铁钙口服溶液中锌铁钙的含量

［摘要］目的建立复方锌铁钙口服溶液中葡萄糖酸锌、葡萄糖酸亚铁、葡萄糖酸钙的含量测定方法。方法样品以硝酸消化,采用火焰原子吸收分光光度法测定。结果该方法的线性、精密度、准确度等均良好。锌、铁、钙的平均回收率分别为99.7%（RSD 1.72%）,99.6%（RSD 0.72%）,100.2%（RSD 1.17%）（n＝9）。结论该方法灵敏快速,准确可靠,可用于复方锌铁钙口服溶液中葡萄糖酸锌、葡萄糖酸亚铁、葡萄糖酸钙的含量测定。     

火焰原子吸收分光光度法用于茶叶中锰含量的测定

目的观察火焰原子吸收分光光度测定茶叶中锰含量的效果。方法称取0.5g茶叶5份,加入不同含量锰标准使用液,采用火焰原子吸收分光光度法测定锰含量。结果测得值1.91～3.03μg,回收率99.5%～100.5%,标准偏差为0.030,相对标准偏差为0.03%。结论火焰原子吸收法测定茶叶中锰含量干扰少,操作简便,精密度,准确度良好。     

原子吸收分光光度法测定磺胺嘧啶银乳膏的含量

目的建立原子吸收分光光度法测定磺胺嘧啶银乳膏含量的方法。方法应用原子吸收分光光度法进行测定,采用标准曲线法计算样品含量。结果样品平均回收率为100.11%,RSD为0.42%。结论该方法准确、精密度高,可作为该药的质量控制方法。     

原子吸收分光光度法测定自制营养液中钾钠镁的含量

目的 建立对自制营养液中钾、钠、镁等含量测定的方法 .方法 分别以氯化钠和氯化锶为消电离剂,采用火焰原子吸收分光光度法测定.结果 钾、钠、镁的平均回收率分别为99.1%,98.5%,100.0%(n＝9),RSD 分别为0.77%,1.51%和0.99%.结论 该方法 的线性、精密度、准确度等均良好.可用于该自制营养液中钾元素、钠元素、镁元素的含量测定.     

原子吸收分光光度法测定磺胺嘧啶银的含量

目的建立原子吸收分光光度法测定磺胺嘧啶银的含量方法。方法应用原子吸收分光光度法进行测定,采用标准曲线法计算样品含量。结果平均回收率为99.89%,RSD=0.21%。结论所用方法准确、精密度高,可作为该药的质量控制方法。     

原子吸收分光光度法测定伤科接骨片中铜的含量简

目的 建立火焰原子吸收分光光度法测定伤科接骨片中铜的含量.方法 采用全自动微波消解系统消解样品,以火焰原子吸收分光光度法检测伤科接骨片中铜元素的含量.结果铜浓度在0～0.8 mg·L-1范围内,具有良好的线性关系,标准曲线方程为A =0.065 889 C -0.000 478 67（r=0.999 9）;方法回收率（n=6）为98.7%.结论采用该法检测伤科接骨片中铜的含量,方法快速、简便,精密度高,重现性好,对伤科接骨片中铜的含量测定具有实际指导意义.     

检测精制肺炎链球菌多糖中甲基戊糖方法的验证

目的 建立检测精制肺炎链球菌多糖中甲基戊糖的方法,并进行方法学验证.方法 将经硫酸和加热处理的精制肺炎链球菌多糖与半胱氨酸盐酸盐进行反应,分别在396 nm和430 nm波长下检测合成的化合物的吸光度值,并根据差值计算甲基戊糖含量.对建立的甲基戊糖测定法进行准确度、专属性、精密度、线性和耐用性验证.结果 该法的准确度良好,甲基戊糖加样回收率为90.2％～108.9％.该法具有较好的重复性和中间精密度,相对标准偏差分别为≤4.6％和1.2％～5.2％,均符合规定的要求.在甲基戊糖质量浓度为2～22 mg/L的检测范围,该法的标准曲线呈现良好的线性,决定系数＞0.99000.该法的专属性较好,精制肺炎链球菌多糖溶液中含有10～50 g/L乙酸钠不会对检测结果产生影响.结论 建立的甲基戊糖测定法可准确定量甲基戊糖含量,可用于对精制肺炎链球菌多糖中甲基戊糖的质量控制.     

优化的α1-抗胰蛋白酶生物活性测定方法的验证

目的 验证优化的α1-抗胰蛋白酶（α1-antitrypsin,α1-AT）生物活性测定方法.方法 用发色底物法测定α1-AT活性,以牛胰蛋白酶替换冻干正常人血清来优化先前建立的方法,验证优化方法的准确性、重复性,并观察不同物质对优化方法的影响.结果 优化方法在胰蛋白酶质量浓度为0.01～0.05 g/L时线性关系良好,相关系数＞0.99.优化方法具有良好的准确性和重复性,当采用优化方法测定质量浓度为0.01、0.03、0.05 g/L胰蛋白酶时,胰蛋白酶的回收率分别为99.33％、94.44％和92.67％,变异系数分别为3.79％、1.66％和1.02％.在一定范围内,聚乙二醇、蔗糖、枸橼酸钠、人白蛋白浓度变化对优化方法测定α1-AT生物活性没有影响.结论 以牛胰蛋白酶作为参考标准品的优化α1-AT生物活性测定方法可用于α1-AT制备工艺中的常规质量控制.     

灵芝孢子粉胶囊中多糖的含量测定

目的：建立灵芝孢子粉胶囊中多糖的含量测定方法。方法：以葡萄糖为标准对照品,采用硫酸-苯酚法测定灵芝孢子粉胶囊中多糖的含量,检测波长为487nm。结果：2.864～11.456μg.mL-1范围内吸光度与被测含量之间呈良好的线性关系,r=0.9995,平均回收率为100.3%。结论：本法准确可靠,重现性好,结果稳定。     

定量伤寒Vi多糖疫苗O-乙酰基含量的药典方法的改良及其验证

目的 通过应用低浓度对照品,对定量伤寒Vi多糖疫苗O-乙酰基含量的药典方法(O-乙酰基测定法)进行改良,并验证该法的可行性.方法 以含0.05、0.10、0.20、0.30、0.40、0.50 μmol溴化乙酰胆碱的对照品溶液制作改良O-乙酰基测定法的标准曲线,并对该法的标准曲线线性、准确度、精密度、专属性和耐用性进行验证.结果 改良O-乙酰基测定法的标准曲线线性良好,决定系数＞0.998.该法的准确度、精密度和专属性良好,O-乙酰基回收率为99.8％～101.3％,实验间和实验内相对标准偏差均＜4％,O-乙酰基加样回收率均＞96％.该法测定O-乙酰基的定量限为0.070 mmol/L.结论 应用低浓度对照品的改良O-乙酰基测定法可用于定量伤寒Vi多糖疫苗O-乙酰基含量.     

Comparison of UV spectrophotometric method and high performance liquid chromatography for the analysis of flunarizine and its application for the dissolution test

This study aimed to develop a simple UV spectrophotometric method for the analysis and the dissolution test of flunarizine in capsules. The UV absorbance was both measured directly and by the first derivative measurements at 254 and 268 nm, respectively. The developed methods were validated for their linearity, accuracy, precision, limit of detection (LOD) and limit of quantitation (LOQ) in comparison with the reported HPLC method. The UV spectrophotometric method illustrated excellent linearity (r2 > 0.9999) in the concentration range of 6-24 microg/mL. Precision (%R.S.D. < 1.50) and recoveries were good (%R > 99.62). The LOD of direct UV and first derivative measurements were 0.09 and 0.84 microg/mL, respectively, and the LOQ were 0.26 and 2.55 microg/mL, respectively. Results from the assay of flunarizine in capsules by the UV spectrophotometric methods, both direct and first derivative measurements were not significantly different from those of the HPLC method (P > 0.05). Additionally, the method was successfully used for the dissolution test of flunarizine capsule and was found to be reliable, simple, fast, and inexpensive.     

Spectrophotometric and AAS determination of ramipril and enalapril through ternary complex formation

Two sensitive, spectrophotometric and atomic absorption spectrometric procedures are developed for the determination of two antihypertensive agents (enalapril maleate and ramipril). The spectrophotometric procedures for the two cited drugs are based on ternary complex formation. The first ternary complex (copper(II), eosin, and enalapril) was estimated by two methods; the first depends on its extraction with chloroform measuring at 533.4 nm. Beer's law was obeyed in concentration range from 56 to 112 microg ml(-1). The second method for the same complex depends on its direct measurement after addition of methylcellulose as surfactant at the pH value 5 at 558.8 nm. The concentration range is from 19 to 32 microg ml(-1). The second ternary complex (iron(III), thiocyanate, and ramipril) was extracted with methylene chloride, measuring at 436.6 nm, with a concentration range 60-132 microg ml(-1). The direct atomic absorption spectrometric method through the quantitative determination of copper or iron content of the complex was also investigated for the purpose of enhancing the sensitivity of the determination. The spectrophotometric and atomic absorption spectrometric procedures hold their accuracy and precision well when applied to the determination of ramipril and enalapril dosage forms.     

Development and validation of a HPLC and a UV derivative spectrophotometric methods for determination of hydroquinone in gel and cream preparations

A high performance liquid chromatographic (HPLC) and a ultraviolet derivative spectrophotometric (UVDS) methods were developed and validated for the quantitative determination of hydroquinone (HQ) in gels and creams containing this compound as a unique active principle. Validation parameters such as linearity, precision, accuracy, specificity, limit of detection (LOD) and limit of quantitation (LOQ) were determined. HPLC was carried out by reversed phase technique on a RP-18 column with a mobile phase composed of methanol and water (20:80, v/v). The linearity in the range of 6.0-30.0 microg/mL present a correlation coefficient (r) of 0.9999, calculated by least square method. The LOD and LOQ were 0.08 and 0.26 microg/mL, respectively. Based on the preliminary spectrophotometric profile of HQ, a signal at 302.0 nm of the first derivative spectrum (1D302.0) was found adequate for validation. The linearity between signal 1D302.0 and concentration of HQ in the range of 10.0-26.0 microg/mL in sulfuric acid (0.1N) present a correlation coefficient (r) of 0.9999. The LOD and LOQ were 0.14 and 0.46 microg/mL, respectively. Statistical analysis by t- and F-tests, showed no significant difference at 95% confidence level between the two proposed methods.     

HPLC测定利巴韦林葡萄糖注射液中5-羟甲基糠醛的含量

目的建立测定利巴韦林葡萄糖注射液中5-羟甲基糠醛含量的高效液相色谱法。方法采用Diamonsil。MC18柱（250mm×4．6mm,5μm）;流动相：甲醇-水（30：70）;检测波长：284nm;流速：1．0mL·min-1;进样量：20儿;柱温：室温。结果利巴韦林和辅料均不干扰5-羟甲基糠醛的检测,加权最小二乘法回归结果表明,在0．0994～7．949μg·mL^-1和0．0020～0．1987μg·mL-1内5-羟甲基糠醛浓度与峰面积均呈现良好的线性关系（r=0．9990和0．9998）,定量限和检测限分别达0．04职和0．012ng,平均回收率为100．4％,RSD为1．8％（n=6）。结论该方法专属性强、灵敏度高、准确性好,适用于利巴韦林葡萄糖注射液中5-羟甲基糠醛的检测。