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。     

蛋黄磷脂中磷脂酰乙醇胺的薄层扫描测定

将超临界ＣＯ２萃取法得到的蛋黄粉中的磷脂经薄层色谱分离，采用双波长薄层扫描仪对其磷脂酰乙醇胺进行测定。平均回收率为９７．６７％，ＲＳＤ为２．３１％。     

新生儿骨矿质含量及影响因素的研究

应用双光子及单光子吸收测定技术，检测了９２名出生３ｄ内的新生儿骨矿质含量，其中巨大儿３０名，正常体重儿３２名，低出生体重儿３０名，其孕龄分别是４０．１±０．７、３９．１±１．５和３７．４±１．２孕周。结果表明，巨大儿、正常体重儿、低出生体重儿的全身骨矿质含量分别是１０１．６±２８．８、８５．２±１９．８、５９．９±２７．２ｇ／ｃｍ２，巨大儿骨矿质含量最高，正常体重儿次之，低出生体重儿最低，差异有显著性（Ｐ＜０．０１）。颅骨、肱骨、股骨的骨矿质含量与全身的骨矿质含量有高度的相关性，相关系数分别是０．９４３、０．８７９和０．７４５（Ｐ＜０．０１）。全身的骨矿质含量与出生体重、孕龄及头围有高度相关性，相关系数分别是０．７５５、０．５９６和０．５５６（Ｐ＜０．０１）。提示颅骨、肱骨及股骨的任一部位均可代表全身的骨矿质含量，肱骨是确定全身骨矿质含量较好的部位，新生儿骨矿质含量受出生体重、孕龄及头围的影响较大。     

Capillary gas chromatographic assay of camphor and m-cresol in dermatological creams

Camphor and m-cresol mixtures are used in antiseptic and anti-itching creams. No compendial method exists for these preparations. This paper reports a capillary gas chromatographic method using FID detection with 2,6-di-tert-butyl-4-methylphenol as internal standard on a 30 m×0.32 mm Supelcowax®-10 column (0.25 μm film) with helium as carrier gas. Ramped temperature programming was applied. The method allows simultaneous quantitation of camphor and m-cresol in the presence of o- and p-cresols, calamine and zinc oxide. Overall percent recoveries (±SD, n=9) of camphor, o-, p- and m-cresol from spiked placebo creams, at a labeled amount of 10 (w/w)% were 96.9±0.6, 98.2±0.6, 99.2±0.5 and 101.0±0.9%, respectively, and at a labeled amount of 1% were 96.7±0.6, 97.8±0.9, 97.8±0.6, and 100.3±1.0%, respectively. The recovery studies were carried out at ±30% of the labeled amounts. Linear peak area or height ratios were obtained (r>0.999) for camphor, o-, p- and m-cresol covering a concentration range of 10–200% of the labeled amount. Linearity (r>0.999) was also obtained for m-cresol when the relative concentration of o- and p-cresol was varied from 5 to 100% of the m-cresol concentration. The resolution between the ‘critical pair’ of p- and m-cresol was ≥1.1. The limit of quantitation was 23 pg for m-cresol and 9.3 pg for camphor using an injection split of 1:50. The repeatability (%RSD) for all compounds were <2% for peak area and <1.4% for peak height ratios. System suitability and robustness of the method were established. The method was successively applied to the assay of available commercial products and allows assay of camphor and the three cresol isomers.