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。     

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.     

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。     

Postmenopausal Women With Colles'' Fracture Have Lower Values of Bone Mineral Density Than Controls as Measured by Quantitative Ultrasound and Densitometry

Measurement of ultrasonographic parameters provides information concerning not only bone density but also bone architecture. We investigated the usefulness of ultrasonographic parameters and bone mineral density (BMD) to evaluate the probability of Colles' fracture. Two-hundred eighty-nine postmenopausal women (62.3 +/- 8.7 yr) with (n = 76) and without (n = 213) Colles' fracture were studied. BMD of lumbar spine and proximal femur was evaluated in all women by dual-energy X-ray absorptiometry (DXA) and speed of sound (SOS), broadband ultrasound attenuation (BUA), and stiffness in the calcaneus were measured by a Sahara ultrasonometer (Hologic). Patients suffering from Colles' fracture had lower values of BMD adjusted by height at the lumbar spine, L2-L4 (0.797 g/cm2 vs 0.860 g/cm2), femoral neck (0.685 g/cm2 vs 0.712 g/cm2 ), SOS (1518 m/sg vs 1525 m/sg), and stiffness (74.6 vs 77.7) (p < 0.05). Nevertheless, BUA values were similar in both groups. After stepwise logistic regression analysis, the area found under receiver operating characteristic (ROC) curves was 0.60 for L2L4 and 0.63 for a formula combining L2L4 and height. Our data suggest that patients suffering from Colles' fracture have lower values of BMD by DXA, SOS, and stiffness. However, the ability of these techniques to discriminate is low because the values for the area under ROC curve are 0.60 for L2-L4 and 0.63 for a formula derived of the combination of L2-L4 and height.     

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％。     

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.     

复方栀子冲剂栀子甙薄层扫描测定

应用薄层扫描法测定了复方栀子冲剂中栀子甙的含量，对实验条件，以正交试验法进行优选，确定了最佳方案，排除了干扰，得到了满意的效果。     

Score Statistic to Test for Genetic Correlation for Proband-Family Design

In genetic epidemiological studies informative families are often oversampled to increase the power of a study. For a proband‐family design, where relatives of probands are sampled, we derive the score statistic to test for clustering of binary and quantitative traits within families due to genetic factors. The derived score statistic is robust to ascertainment scheme. We considered correlation due to unspecified genetic effects and/or due to sharing alleles identical by descent (IBD) at observed marker locations in a candidate region. A simulation study was carried out to study the distribution of the statistic under the null hypothesis in small data‐sets. To illustrate the score statistic, data from 33 families with type 2 diabetes mellitus (DM2) were analyzed. In addition to the binary outcome DM2 we also analyzed the quantitative outcome, body mass index (BMI). For both traits familial aggregation was highly significant. For DM2, also including IBD sharing at marker D3S3681 as a cause of correlation gave an even more significant result, which suggests the presence of a trait gene linked to this marker. We conclude that for the proband‐family design the score statistic is a powerful and robust tool for detecting clustering of outcomes.     

定量组织速度成像对右室起搏患者左室收缩运动的研究

目的　应用定量组织速度成像 (QTVI)评价右室心尖起搏 (RVAP)VVI型对左心收缩功能的影响。方法　应用GEVivid 7彩色多普勒超声显像仪对 2 0例RVAP患者和 2 0例正常人的心尖四腔切面的室间隔和左室外侧壁速度和位移曲线进行观察 ,测量心电图Q波分别至室间隔和左室外侧壁收缩期峰速度的时间 ,并除以R R间期进行校正。结果　QTVI显示右室起搏器置入者的室间隔与左室外侧壁速度曲线的收缩期S波非同步出现。Q波至室间隔收缩期峰速度的时间短于Q波至左室外侧壁收缩期峰速度的时间 ,两者分别为 ( 0 .12± 0 .0 2 )s和 ( 0 .14± 0 .0 2 )s,P <0 .0 5。结论　右室起搏后早期的左室整体收缩功能虽未见明显下降 ,但QTVI可以发现室间隔与左室壁收缩明显的不协调 ,可作为早期分析左室收缩运动的定量方法。