HPLC法测定复方甲苯咪唑片中甲苯咪唑和盐酸左旋咪唑的含量

目的：建立高效液相色谱法同时测定复方甲苯咪唑片中甲苯咪唑和盐酸左旋咪唑的含量。方法：用十八烷基硅烷键合硅胶为填充剂;流动相为0．05mol·L-1磷酸二氢钾溶液-甲醇（40：60）,流速为1．0mL·min-1,检测渡长为230nm。结果：甲苯咪唑和盐酸左旋咪唑的线性范围分别为42．24—168．96mg·L-1（r=0．9998）和10．56～42．24mg·L-1（r=0．9996）。结论：本文建立的高效液相法结果准确可靠,可作为复方甲苯咪唑片中甲苯咪唑和盐酸左旋咪唑的含量测定方法。     

GC测定甲苯咪唑中的残留溶剂

目的 采用顶空气相色谱法测定甲苯咪唑原料药中的有机溶剂残留量。方法 以DMF-H₂O（2︰1）溶液为样品溶剂,选用PerkinElmer气相色谱仪,配备顶空进样器和FID检测器,Agilent DB-624毛细管柱为分析柱,外标法测定。结果 甲醇、乙醇、异丙醇、三氯甲烷和甲苯分别在18.7~224,46.9~562,46.9~562,1.50~17.9,2.81~33.8 μg·mL^-1内线性关系良好（r>0.999）;各组分检出限分别为0.19,0.10,0.11,0.18,0.08 μg·mL^-1;各组分回收率为90.0%~110.0%。结论 该方法准确、灵敏、可靠,可用于甲苯咪唑有机残留溶剂的测定。     

高效液相色谱法测定盐酸左旋咪唑片的含量

目的 以西咪替丁为内标,建立RP-HPLC法测定盐酸左旋咪唑片的含量。方法 选用ODS-C₁₈柱(5μm,4.6mm×150mm);流动相:甲醇-水-二乙胺-磷酸(36∶64∶0.1∶0.06),pH7.0;检测波长:215nm;流量∶1.0ml·min^-1;进样体积∶20μl。结果 进样量在0.32～1.6μg范围内,相关性良好,回归方程:Y=22.01X+7.4×10^-3,r=0.9998。平均回收率为99.8%(n=5)。结论 本法简便、快速、准确。     

HPLC法测定复方甲苯咪唑片中甲苯咪唑和左旋咪唑的含量

采用 C8 不锈钢柱 ,以甲醇 - 0 .5%醋酸铵作流动相 ( p H=5.0 ) ,检测波长 2 2 0 nm,多潘立酮作为内标物 ,峰面积比定量。结果 :该方法回收率甲苯咪唑 98.80 % ( RSD =1 .2 4 % ) ,盐酸左旋咪唑 99.37% ( RSD= 0 .77% )。     

丸剂中非法添加环丙沙星的快速检测方法研究

目的 建立一种丸剂中非法添加环丙沙星的快速检测方法。方法 通过¹⁹F-核磁共振定量（¹⁹F-qNMR）法对添加入当归苦参丸中的环丙沙星进行检测,以4,4’-二氟二苯甲酮为内标,以氘代DMSO为溶剂,采集δ-120.3处环丙沙星信号和δ-104.8处内标信号面积,计算环丙沙星的含量。结果 以环丙沙星和内标信号面积比为纵坐标,环丙沙星和内标质量比为横坐标,得到线性回归方程为：Y=3.384 1X+0.114 8,R²=0.992,环丙沙星在5～30 mmol/L具有良好的线性,检出限为7.798×10^-2 mg/mL,定量限为0.260 mg/mL。建立的¹⁹F-qNMR法精密度、重复性、稳定性、加样回收率均符合检测要求。结论 所建立的¹⁹F-qNMR法样品制备简单,检测时间短,灵敏度高,适合对丸剂中非法添加的环丙沙星进行含量测定。     

Nafion修饰玻碳电极测定微量左旋咪唑的研究

以玻碳电极为基体,制备了nafion修饰电极,研究了非电活性阳离子药物左旋咪唑在该电极上的测定方法及作用机理。将左旋咪唑加到含电活性阳离子药物多巴胺的电解质溶液中,使多巴胺峰电流下降,峰电流的降低与左旋咪唑的浓度对数在2×10^-6～8×10^-5mol·r^-1范围内呈良好线性关系,本方法的检测下限为1×10^-6mol·L⁶,回收范围为96.8%～105.8%,相对标准偏差为3.2%(n=10)。     

赛拉嗪对麻醉大鼠海马CA1区乙酰胆碱含量的影响

应用乙酰胆碱选择性微电极技术,观察到小剂量赛拉嗪(2.0和6.0mg·kg^-1)可显著增加大鼠海马CA1区ACh的含量,而大剂量赛拉嗪(10.0mg·kg^-1)及咪唑克生(0.6mg·kg^-1)则作用相反。咪唑克生虽可明显拮抗赛拉嗪的作用,但海马CA₁区ACh的含量仍显著低于正常水平。在去兰斑核的大鼠上,赛拉嗪(2.0和6.0mg·kg^-1)及咪唑克生(0.6mg·kg^-1)分别对海马CA₁区ACh的含量具有减少和增加作用,且咪唑克生拮抗赛拉嗪的作用后,海马CA₁区ACh的含量基本恢复至正常水平。结果提示,赛拉嗪对麻醉大鼠海马CA₁区ACh含量呈双相性影响,咪唑可生虽能显著拮抗赛拉嗪的作用,但海马CA₁区ACh的含量仍明显低于正常水平,可能分别与赛拉嗪和咪唑克生降低或提高中枢NE能系统的功能有关。     

O/W型甲苯咪唑口服乳剂兔体内药物动力学研究

对甲苯咪唑口服乳剂在免体内的药物动力学进行研究。方法：以阿苯咪唑为内标,采用反相高效液相色谱法测定血中的甲苯咪唑浓度。流动相为：甲醇-0．01mol·L－1硫酸接缓冲浪（58：42）;流速：1ml·min-1;检测器波长：247nm。结果：标准曲线为：C（μg·ml-1）=0．6026Ai/As－0.6597（r＝0、9929）;线性范围为4.996～999．2ng·ml-1,平均回收率为（97．8±5．4）％,RSD＝5．52％。方法的精密度和重现性符合生物样品测定要求。甲苯咪唑乳剂在兔体内的AUC比片剂高出四倍还多,其它药物动力学参数如Cmax,Kat1/2（Ka）,Cls,Vd等均与片剂间差异有显著性（P＜0.05）。结论：甲苯咪唑乳剂与片剂相比,吸收快,Cmax和AUC均高,为临床应用提供参考。     

《中国药典》2010年版盐酸头孢吡肟红外鉴别存在的问题及修订建议

《中国药典》2010年版二部盐酸头孢吡肟〔鉴别〕(2)项下规定"本品的红外光吸收图谱应与对照的图谱(光谱集1184图)一致"。我们对某药业有限公司购进的盐酸头孢吡肟进行红外鉴别检验时,发现在2 600～3 200 cm^-1范围内波形不相符,特别是在约2 850 cm^-1,2 910 cm^-1波数处吸收峰差距大。     

盐酸左旋咪唑和甲苯咪唑的致突变性试验研究

盐酸左旋咪唑和甲苯咪唑均为抗肠道蠕虫类药物。本实验根据我国新药审批的有关要求来检测这二类药物的致突变作用,该实验通过诱发CHL 细胞染色体畸变的体外试验和小鼠骨髓细胞染色体的体内试验这两条途径来检测。实验结果表明:在体内试验中,甲苯咪唑(400-1600mg/kg)与阴性对照组(N.S)相比,有非常显著性差异(p<0.01);在体外试验中,甲苯咪唑(0.39-0.78μg/ml)培养24h 和48h 对CHL 细胞所诱发的染色体变化率显阳性。说明甲苯咪唑具有损伤小鼠骨髓细胞染色体和诱发CHL 细胞染色体畸变的遗传物质存在。而盐酸左旋咪唑的体内、体外试验显示阴性。     

Quantitation of pharmaceutically important phenothiazines by oxidimetry

A new spectrophotometric method for the assay of phenothiazines in pure form as well as in pharmaceutical formulations with the chromium(VI)-metol-sulfanilic acid system has been developed. The method is based on the oxidation of the drugs by a known excess of chromium(VI) and subsequent determination of the unreacted oxidant by interacting with metol and sulfanilic acid. The reacted oxidant corresponds to the drug content. The coloured species exhibits maximum absorbance at 530 nm. Beer's law is obeyed over the concentration range 5-60 micrograms ml-1 and the relative standard deviation is found to be less than 2%. The apparent molar absorptivities are in the range 3.77 x 10(3)-3.98 x 10(3) l mol-1 cm-1, the detection limits being in the range 0.6133-1.1349 micrograms ml-1. The method was successfully applied to the determination of the studied drugs in their formulations and the mean percentage recoveries were found to be 97.32-102.80%.     

高效毛细管电泳法同时测定红花中腺苷、芦丁和槲皮素的含量

目的 用高效毛细管电泳法对红花中的有效成分腺苷、槲皮素和芦丁同时进行含量测定。方法 采用熔融石英毛细管柱（66.5 cm×50 μm ID，有效长度58 cm）作为分离通道；以50 mmol·L^-1硼砂其中含18%甲醇的溶液（pH 9.7）为运行缓冲液；运行电压: 24 kV；毛细管柱温: 20 ℃；检测波长： 210 nm。结果 以利福平为内标，腺苷、芦丁和槲皮素分别在10～160 mg·L^-1，100～2 000 mg·L^-1和100～1 600 mg·L^-1 线性关系良好（R>0.998）；平均回收率分别为98.5%～100.5%， 96.9%～99.5%和99.1%～99.5%； RSD分别为6.5%，5.2%和5.6%(N=5)。结论 此法操作简便快速，回收率及重现性好，可作为红花质量控制的方法。     

Liquid chromatographic procedure for the quantitative analysis of megestrol acetate in human plasma

A simple, sensitive, and reproducible high-performance liquid chromatographic (HPLC) procedure was developed for the quantitative analysis of megestrol acetate in human plasma. An internal standard, 2,3-diphenyl-1-indenone, was added to 0.5 mL of plasma followed by extraction with hexane. The residue remaining after evaporation of hexane was reconstituted in methanol and injected onto a mu-Bondapak C18 column. The column was eluted with acetonitrile:methanol:water:acetic acid (41:23:36:1), and the eluant was monitored at 280 nm. Megestrol acetate and the internal standard eluted at 6-7 and 12-14 min, respectively. The peak height ratio (megestrol acetate/internal standard) versus plasma concentration was linear over a range of 10-600 ng of megestrol acetate/mL of plasma, and the limit of detection was 5 ng/mL. The mean intra- and interassay accuracies were within 3% of the actual values. The mean intra- and interassay precision, as estimated by RSD, were 4 and 6%, respectively. Constituents in human plasma and megestrol, a possible degradation product, did not interfere in the assay. The procedure was applied to the analysis of plasma samples from subjects receiving 40 mg of Megace q.i.d.     

高效液相色谱法测定人血浆和脑脊液中左氟沙星浓度及药代动力学研究

目的旨在测定左氟沙星药代动力学。用RP-HPLC法,以环丙沙星为内标,反相C₁₈为分析柱,10mmol·L^-1磷酸二氢钾—10mmol·L^-1溴化四丁铵—乙腈(45∶45∶10)为流动相,磷酸调至pH3.0,检测波长295nm,测定血浆和脑脊液中左氟沙星浓度,平均回收率分别为74.76%和82.43%,日内日间误差小于5%,最低检测浓度血浆10μg·L^-1,脑脊液6μg·L^-1。10名开颅手术病人单次口服左氟沙星片300mg的血液和脑脊液药代动力学特征均符合开放性一室模型。     

Thermodynamic and kinetic characterization of polymorphic transformation of famotidine during grinding

Two polymorphs of famotidine were prepared by recrystallization from acetonitrile for form A and methanol for form B, respectively. The effect of grinding process on the polymorphic transformation of famotidine was investigated. Each famotidine sample ground for various grinding times in a ceramic mortar was determined by differential scanning calorimetry (DSC), conventional and thermal Fourier transform infrared (FT-IR) microspectroscopy. The results indicate that the raw material of famotidine was proved to be a form B. A unique IR absorption band at 3505 cm(-1) for famotidine form B gradually decreased its intensity with the grinding time, while two newer IR absorption bands at 3451 and 1671 cm(-1) for famotidine form A slowly appeared. The peak intensity ratio of 3451/350 5 cm(-1) was linearly (r=0.9901) increased with the grinding time, suggesting that the grinding process could induce the polymorphic transformation of famotidine from form B to form A by a zero-order process. The DSC endothermic peaks also confirmed this polymorphic transformation from famotidine form B (167 degrees C, DeltaH: 165J/g) to famotidine form A (174 degrees C, DeltaH: 148J/g) in which the values of enthalpy were linearly reduced with the increase of grinding time (r=0.9943). The phase transition temperature of the different ground famotidine samples could be easily and only evidenced by using thermal FT-IR microspectroscopy, rather than by DSC analysis. These phase transition temperatures of the famotidine form B ground for 5-20 min quickly reduced from 144 to 134 degrees C and maintained a constant at 134 degrees C even after 20-30 min grinding. The grinding process not only decreased the crystallinity of famotidine form B but also reduced the particle size of famotidine form B, resulting in easy induction of the polymorphic transformation of famotidine from form B to form A in ground famotidine sample.     

反相高效液相色谱法测定血液中去甲万古霉素浓度的研究

目的：建立去甲万古霉素血药浓度的反相高效液相色谱（RP －HPLC）测定法。方法以替硝唑或甲硝唑为内标,血液样品处理采用15％ HClO4沉淀、高速离心,NH4 Ac 溶液稀释后进样。色谱分析使用 Kromasil C18柱（150 mm ×4．6 mm,5μm）,流动相组成为甲醇—乙腈—40 mmol·L －1 KH2 PO4缓冲液（含0．1％磷酸）＝15∶5∶80（v／v）,进样量为20μL,流速为1．0 mL· min －1,柱温35℃,紫外检测波长236 nm。灵敏度 AUFs ＝0．02,以峰面积、内标法定量。结果该法在去甲万古霉素浓度（X）为5．0～160 mg·L －1间呈良好线性关系,相关系数 r ＝0．9985（n ＝6）,血清最低检测浓度为2．5 mg·L －1（S ／N≥3）,日内、日间 RSD ＜10％,一个月内、反复冻融后的稳定性考察 RSD ＜10％。结论此法快速、简便、灵敏、可靠,适用于去甲万古霉素血药浓度监测。     

A sensitive spectrophotometric determination of acetaminophen.

A sensitive, accurate and precise spectrophotometric method is described for the determination of Acetaminophen (paracetamol, ACTP) in pure form and in pharmaceutical formulations. The principle of the method is the reduction, of Fe(III) to Fe(II) by the ACTP in the presence of o-Phenanthroline (o-Phen), when the orange-red coloured chelate complex [Fe(II)-(o-Phen)3]2+ the ferroin complex was formed, and its absorbance was measured at lambda = 510 nm. The apparent molar absorptivity, referred to ACTP was 3.16 x 10(4) 1 mol-1 cm-1 and the Sandell's sensitivity was calculated as 4.8 ng cm-2. The calibration graph was rectilinear over the range 0.25-10.0 ppm of ACTP and the regression equation was calculated as A = 2.06 x 10(-1) C + 4.78 x 10(-3) with a correlation coefficient of 0.9999 (n = 8). A statistical analysis by means of the Student's t-test as well as by the variance ratio F-test, indicates that the proposed new method is equivalent to the corresponding B. P. 1988 and U. S. P. XXII official methods with regard to accuracy and precision.     

Spectrophotometric determination of paracetamol in pure form and in tablets

A spectrophotometric method is proposed for the determination of paracetamol in pure form and in tablets. The method depends on reaction of the drug with ammonium molybdate in strongly acidic medium to produce molybdenum blue. Effects of variables such as temperature, heating time, acidity and reagent concentration have been evaluated to permit selection of the most advantageous technique. Beer's law was followed for concentrations of up to 6 micrograms ml-1 of paracetamol and the detection limit (p = 0.05) was 0.10 microgram ml-1. The molar absorptivity at 670 nm was 2.6 x 10(4) l mol-1 cm-1 and the relevant Sandell's sensitivity of the reaction was 0.0059 microgram cm-2 per 0.001 absorbance unit. Statistical analysis of the results and comparison with results by the BP method of analysis are also reported.     

Reaction of sodium amoxicillin with Cu(II) ion in a methanolic medium.

The present article considers several physicochemical aspects of the complexation reaction of sodium amoxicillin and Cu(II) ion in a methanolic medium. Analysis of spectrophotometric data demonstrated the formation of two complex species with amoxicillin:Cu(II) ion mole ratios of 1:1 and 2:1. Stability constants (beta) and molar absorptivities at 610 nm (epsilon) of the complexes (20 degrees C) in methanol were calculated simultaneously by a computer program on the basis of absorbance data obtained at 610 nm. The values thus calculated for the 1:1 complex were as follows: log beta 1 = 5.48 +/- 0.21 L.mol-1, epsilon 1 = 70 +/- 2 L.mol-1.cm-1. The values for the 2:1 complex were as follows: log beta 2 = 8.98 +/- 0.17 L2.mol-2 and epsilon 2 = 138 +/- 4 L.mol-1.cm-1. The amoxicillin:Cu(II) ion complexes were quite stable over time.     

2-脱氧链霉胺取代衍生物的结构确证和1H核磁定量

对新型氨基糖苷类抗生素合成中(本文阐述的是阿米卡星合成中的2个中间体,而非新型氨基糖苷类抗生素)的两个重要中间体进行结构确证和核磁定量。采用13C NMR、1H NMR、1H 1H-COSY、HMBC和MS对化合物1和化合物2进行了结构确证,并分别以马来酸和甲酸钠为内标物、D2O为溶剂,通过比较马来酸δ6.23ppm内标峰和化合物1δ5.05ppm、δ5.66ppm定量峰面积,以及甲酸钠δ8.36ppm内标峰和化合物2 δ2.00ppm、δ5.72ppm定量峰面积计算化合物1和化合物2的含量。化合物1为3-氨基-3-脱氧-α-D-葡吡喃糖基-(1→6)-[2,3,4,6-四脱氧-2,6–二氨基-α-D-赤式-己吡喃糖基-(1→4)]-1-N-[(2S)-4-氨基-2-羟基-1-氧丁基]-2-脱氧-D-链霉胺,化合物2为3-氨基-3-脱氧-α-D-葡吡喃糖基-(1→6)-[2,3,4,6-四脱氧-2,6–二氨基-α-D-赤式-3-烯-己吡喃糖基-(1→4)]-1-N-[(2S)-4-氨基-2-羟基-1-氧丁基]-2-脱氧-D-链霉胺,化合物1和化合物2的含量分别为64.98%和75.38%。化合物1和化合物2是2-脱氧链霉胺取代衍生物,采用氢核磁共振内标法可快速、准确地型氨基糖苷类抗生素合成过程中无商品化标准品的重要中间体进行定量分析。