吉非罗齐中有机溶剂残留量的顶空毛细管GC测定

建立了顶空毛细管GC法测定吉非罗齐中甲酸乙酯、THF和甲基环己烷3种有机溶剂的残留量。采用HP-1毛细管柱，溶剂DMA，内标乙酸乙酯。平均同收率分别为99．8％、100．3％、100．0％，RSD分别为0．71％、1．51％和1．76％。     

枳椇子总黄酮提取工艺及其解酒作用

分别用水和乙醇作为溶剂加热提取枳椇子中的总黄酮,用比色法测定黄酮的含量,分别以提取时间、加热温度、料液比、提取次数等因素进行正交试验.对两种提取方法进行比较,确定各因素对提取效果的影响并对其解酒作用进行研究.水提取法的最优条件是：100 ℃,料液比1 g：8 mL,加热0.5 h,回流提取3次;醇提取法的最佳条件：80 ℃,料液比1 g：6 mL,加热1.5 h,以体积分数50%的乙醇回流提取3次.实验结果显示,醇提取法比水提取法效果更好,枳椇子提取液具有一定的解酒作用.     

GC法测定金银三七胶囊中的冰片的含量

目的：建立金银三七胶囊中冰片的含量测定方法。方法：采用GC法，色谱柱为10％PEG-20M；FID氢火焰检测器：柱温为115℃。结果：冰片在0．02559-0．5118μg范围内线性良好。加样回收率为99．9％，RSD％为1．94％（n=9）。结论：方法简便，可行，重现性良好，结果准确，可加强金银三七胶囊的质量控制。     

Comparison between a swim-up and a Percoll gradient technique for the separation of human spermatozoa

Two methods of separating human sperm were compared using twenty-two semen samples. The sperm were separated by a swim-up technique or by self-migration on a Percoll gradient followed by medium change. After separation, the sperm obtained were assessed for progressive motility, ATP content, energy charge index ([ATP + 0.5 ADP]/[ATP + ADP + AMP]) and morphology. In general, and especially for semen samples containing less than 20 X 10(6) sperm/ml, separation by Percoll gradient selected sperm that were superior to those separated by the swim-up technique. The relatively high energy charge index (greater than 0.8) showed that the sperm tolerated the separation conditions well. It is suggested that self-migration on a Percoll gradient should prove useful for obtaining sperm of high quality.     

Fluorimetric assay of rufloxacin in serum and in pharmaceutical formulations

A simple and rapid fluorimetric method for the determination of 9-fluoro-10-[N-(4′-methyl)piperazinyl]-7-oxo-2,3-dihydro-7H-pyrido[1,2,3-d,e][1–4]benzothyazin-6-carboxylic acid hydrochloride (MF 934), in serum and in pharmaceutical formulations, has been developed based on its strong fluorescence, in 0.1 N H₂SO₄, at 526 nm (excitation wavelength at 340 nm). The procedure which involves the direct dilution of the sample requires only a few minutes and the sample volume is only 20–100 μl of serum, depending on the drug concentration. Tedious sample preparation procedures such as extraction, deproteinization, or centrifugation are not necessary. The minimum concentration that can be detected is 0.3 ng ml⁻¹, the standard curve in 0.1 N H₂SO₄ was found to be linear from 0.005 to 1.5 μg ml⁻¹ and from 0.01 to 0.07 g in plasma after dilution with 0.1 N H₂SO₄.     

Comparison of assays for determination of peptide content for lyophilized thymalfasin*

Abstract: Precise determination of the peptide content in drug substance samples depends highly upon the particular peptide compound and methodology used. Four independent methods were evaluated and compared to determine which would produce the best experimental precision for analysis of thymalfasin (thymosin α‐1). Four different methods were evaluated including elemental analysis (CHN), quantitative amino acid analysis (AAA), high‐performance liquid chromatography (HPLC), and Kjeldahl. This study demonstrates that the AAA method is highly variable in one laboratory while quite precise in another laboratory. Similarly, HPLC results depended on the laboratory conducting the study with more precise values obtained under cGMP. On the contrary, the CHN method yielded highly precise [i.e. <2% coefficient of variation (CV)] values. As precise knowledge of protein content is fundamental for the compounding of final pharmaceutical product of a specific potency, the CHN analysis is recommended for peptide content determination of the drug substance thymalfasin.     

Bone growth patterns in Chinese children and adolescents: a 6-year follow-up study provides evidence for sexual dimorphism and tracking

Summary We prospectively examined bone growth patterns in 894 children aged 6–17 years at the baseline visit, with a 6-year follow-up. Results show bone “tracking” over a six-year interval and sexual dimorphism of bone attained levels and timing of peak bone growth. Our findings underscore childhood and adolescence as critical periods for building bone and developing gender differences. Introduction Bone growth patterns were prospectively examined in 894 Chinese children (496 males), aged 6–17 yrs, from a population-based twin cohort. Whole-body bone area (BA), bone mineral content (BMC), and bone mineral density (BMD) were measured by DEXA at baseline and a 6-yr follow-up. Methods Graphic smoothing plots and generalized estimating equations were used to model bone attained levels, growth, and “tracking”. Results Attained levels of BMC and BA increased curvilinearly with age. Male attained levels were higher than females after age ∼15 yr, but BMD was lower between 13–17 yrs (Tanner stage I to IV). In both genders, peak BMC and BMD growth lagged ∼2 yrs behind peak BA growth, which lagged 2 yrs behind peak height growth. Peak bone growth occurred 1–3 yrs later in males. Over the 6-yr follow-up, all bone measurements “tracked”, but “shifting” across ranks also occurred, and baseline tertile ranking influenced bone growth. Females with early menarche had higher attained levels than females with late menarche at age 12–13 yrs. Conclusion Our findings confirm and expand previous studies on peak bone growth conducted in Caucasian cohorts, particularly sexually dimorphic and maturational effects. The significant “tracking” of bone measurements in this 6-yr follow-up study underscores the importance that osteoporosis prevention should begin in childhood and adolescence. Fengxiu Ouyang and Binyan Wang contributed equally to this article. Source(s) of support: This study is supported in part by grant R01 HD049059, R01 HL0864619 and R01 AR045651 from the National Institute of Health and by the Food Allergy Project.     

灵芝菌合剂中灵芝多糖含量的测定

目的：探讨灵芝菌合剂中灵芝多糖含量的检测方法。方法：采用分光光度法，以无水葡萄糖为对照品，检测波长为490nm。结果：此方法在0～120μg范围内线性关系良好，灵芝多糖的平均回收率为99．09%。RSB为1．14％。结论：本法简便快捷，准确度高，重现性好，可作为本制剂的质控方法。     

接触镜与泪液形态关系的临床评价

目的 :观察配戴不同种类接触镜后眼表面泪膜的形态、稳定性及泪液量的变化。方法 :对日戴SCL、RGPCL和Ortho KCL的 2 14名近视患者 4 2 8只眼 ,利用表面泪膜观察装置 (DR 1)观察戴镜前后眼表泪液膜和戴镜状态下镜上泪液膜的形态分级 ,同时测定泪膜破裂时间 (BUT)。利用酚红染色棉丝测定SCL戴镜前后的泪液量 ,并用折射仪 (AtagoCL 1)测量SCL含水量的变化。结果 :SCL配戴者随戴镜时间延长 ,BUT明显缩短 (P <0 .0 1) ,RGPCL和Ortho KCL配戴者戴镜 5年以内 ,BUT无明显变化 (P >0 .0 5 )。戴镜后RGPCL ,Ortho KCL和非戴镜正常眼三组间眼表泪膜分级比例差异无显著性 ,SCL组Ⅰ级比例为 6 .5 % ,显著低于其他组(16 .1%～ 2 3.0 % )。镜上泪膜 ,SCL、RGPCL和Ortho KCL三组均以Ⅳ级为主 (分别占 5 4 .4 %、5 3.4 %和 5 1.5 % ) ,SCLⅠ级比例仅 1.9% ,显著低于另二组 (分别占 6 .2 %和 12 .4 % )。SCL配戴者随戴镜时间延长 ,泪液量轻度减少 ,SCL含水量在戴镜 1w后即显著降低。结论 :科学配戴接触镜对泪液膜质量无明显影响 ,但SCL长期使用可能对泪膜有一定干扰作用。