毛细管气相色谱法测定坎地沙坦酯原料药中8种有机溶剂残留量

目的:建立测定坎地沙坦酯原料药中8种有机溶剂甲醇、乙醇、乙腈、丙酮、乙醚、二氯甲烷、乙酸乙酯与四氢呋喃残留量的方法。方法:采用气相色谱法。色谱柱为Agilent HP-5毛细管柱,以(5%)苯基-(95%)甲基聚硅氧烷为固定液,柱温采用程序升温,氢火焰离子化检测器温度为250℃;载气为高纯N2;顶空进样,加热温度为100℃,加热时间为30 min。结果:8种有机溶剂在各自的检测质量浓度范围内线性关系良好(r=0.999 6⁰.999 9),平均回收率均为99.6%0.999 9),平均回收率均为99.6%¹00.3%(RSD=0.89%100.3%(RSD=0.89%¹.98%,n=3);定量限分别为0.09、0.15、0.12、0.3、0.6、0.18、0.45、0.21 ng;检测限分别为0.03、0.05、0.04、0.1、0.2、0.06、0.15、0.07 ng。样品中只检出了丙酮。结论:建立的方法操作简便、精密度高,可有效控制坎地沙坦酯原料药中残留的8种有机溶剂。     

2种测定抗菌药物水分方法的比较研究

目的 采用气相色谱法和费休氏法测定抗菌药物中水分的含量,探讨使用气相色谱法测定抗菌药物水分含量的可行性。方法 气相色谱法采用顶空毛细管气相色谱-热导检测器法进行测定,使用Agilent HP-PLOT/Q毛细管色谱柱（30 m×0.530 mm×40 μm）,载气为高纯氦气,流量3 mL·min^-1,进样量250 μL,分流比20：1,进样口温度为200℃;柱升温程序：初始温度150℃,保持6 min,以60℃·min^-1的速率升到250℃,保持5 min;热导检测器温度为250℃,电流为70 mA。费休氏法采用中国药典2015年版四部通则0832中水分测定第一法中的容量滴定法。结果 除了注射用头孢曲松钠和注射用头孢唑肟钠外,其他抗菌药物样品2种测定方法测定结果无显著性差异。结论 本研究所建立的气相色谱法,可用于部分抗菌药物水分含量的测定。     

Phenolic composition and radical scavenging activity of commercial Greek white wines from Vitis vinifera L. cv. Malagousia

Seven commercial white wine samples of the Malagousia cultivar were investigated for the first time with regard to their phenolic composition and radical scavenging activity. Total phenol content, corrected for ascorbic acid contribution (0–47 mg gallic acid equivalents/L of wine), ranged between 241 and 336 mg gallic acid equivalents/L of wine. On the other hand, the range for total hydroxycinnamates was 51.5–122.4 mg chlorogenic acid equivalents/L of wine and that for total flavanols 19.6–68.8 mg catechin equivalents/L wine. Fifteen phenolic compounds were identified and quantified by gas chromatography/mass spectrometry in the selective ion monitoring and high-performance liquid chromatography coupled with diode array detector. Tyrosol, caftaric, caffeic and 2-S-glutathionyl caffeoyl tartaric (GRP) acids were the major phenolics in all samples with mean concentrations of 12.32, 10.71, 10.17 and 4.79 mg/L wine, respectively. Catechin (3.75 mg/L) and p-coumaric acid (3.04 mg/L) followed in abundance. Variations in the values of GRP/caftaric (0.1–4.6) and caffeic/caftaric (0.4–4.2) acid concentrations, suggested differences in the degree of oxidation on one hand and hydrolytic processes during production and bottling on the other. Despite these variations, the radical scavenging activity of samples examined with DPPH and ABTS⁺ assays (mean value 0.85 and 3.45 mmol Trolox equivalents/L of wine) indicated a high efficiency in comparison to literature data on native and foreign white wines. The present findings can be useful for both technological and nutritional purposes.     

气相色谱法测定盐酸美金刚片的含量

建立了测定盐酸美金刚片含量的气相色谱(GC)方法。方法采用Agilent DB-225 (30m*0.53mm,1.0μm)毛细管色谱柱,以氮气为载气,流速5mL.min-1,柱温：110℃,进样口温度：250℃,进样量：2.0μL。火焰离子化检测器(FID),检测器温度：250℃。以盐酸金刚乙胺作为内标物测定盐酸美金刚片的含量。盐酸美金刚在0.157 8mg.mL-1～0.480 6mg.mL-1范围内与峰面积呈现良好的线性关系(r=0.999 0)。所建立的方法准确、回收率较为理想,可用于盐酸美金刚片含量的测定。     

复方毛冬青注射液中甲基正壬酮的含量测定

目的:为复方毛冬青注射液建立专属性含量测定方法。方法:采用气相色谱法对甲基正壬酮进行含量测定。色谱柱:HP-1(Aglient 19091z-413,30 m×320μm×0.25μm);氮气为9.23 psi,流量1.8 mL/min;空气400 mL/min;氢气40 mL/min;柱温80℃(2 min)至220℃,升温速率为15℃/min;再升至270℃(13.75 min),升温速率为40℃/min;汽化室240℃;检测室280℃;进样量1μL;检测器为FID。结果:线性范围为1.0~20.0μg/mL,平均回收率为99.05%,RSD=1.29%(n=6)。结论:本法操作简单、可靠、具有实用性。     

抗湿热胶囊对热损伤大鼠下丘脑-垂体-肾上腺皮质系统的影响

目的 通过研究抗湿热胶囊对热损伤大鼠下丘脑-垂体-肾上腺系统的影响,探究其抗热损伤的作用机制。方法 采用人工气候箱制成高温高湿环境,造成热损伤模型,测定大鼠下丘脑、垂体、血浆中β—EP、GC和ACTH的含量。结果 给药组大鼠热损伤后血浆和下丘脑中B—EP的含量高于模型组（P〈0．05）;GC和ACTH的含量也都有所增加,给药组GC的含量高于模型组（P〈0．05）。结论 抗湿热胶囊能明显抑制热损伤大鼠体温升高,其机制可能是通过增强下丘脑-垂体-肾上腺系统对机体的调节和代偿作用,来提高机体的耐受力,减轻热损伤。     

The impact of age on prognosis in patients with gastric cancer: experience in a tertiary care centre

BackgroundGastric cancer (GC) is a leading cause of cancer-related death in the world and most patients have advanced disease upon presentation. The effect of age on prognosis in GC is controversial. We aimed to determine the impact of age on survival in patients with GC.MethodsThis was a retrospective study of the medical records of Lebanese patients diagnosed with GC at the American University of Beirut Medical Center (AUBMC) between 2005 and 2014. Patients were divided into young (<65 years) and older groups (≥65 years). A multivariate analysis was done to determine the independent predictors of survival. Kaplan-Meier method was used for analysis of long-term survival outcomes.ResultsThe sample consisted of 156 patients. The mean age was 62.15 (SD 13.54). Most patients presented with stage 4 disease (62.2%) and poorly differentiated histology (66.4%). The most common symptoms were abdominal pain and weight loss. On bivariate analysis, advanced stage (P=0.02) and higher grade (P=0.04) were associated with increased mortality. Patients <65 years of age were significantly more likely to have poorly differentiated tumours, while patients ≥65 years had more comorbidities (P=0.001). The 5-year DFS were 35% and 37% for patients <65 years of age and ≥65 years of age, respectively (P=0.15).ConclusionsHigher grade and advanced stage are associated with worse survival in patients with GC, but age did not seem to have an impact. Screening high risk patients and early diagnosis are necessary to improve survival.     

Haplotypes in the GC,CYP2R1 and CYP24A1 Genes and Biomarkers of Bone Mineral Metabolism in Older Adults

Candidate gene studies have analyzed the effect of specific vitamin D pathway genes on vitamin D availability; however, it is not clear whether genetic variants also affect overall bone metabolism. This study evaluated the association between genetic polymorphisms in GC, CYP2R1 and CYP24A1 and serum levels of total 25(OH)D, iPTH and other mineral metabolism biomarkers (albumin, total calcium and phosphorus) in a sample of 273 older Spanish adults. We observed a significant difference between CYP2R1 rs10741657 codominant model and total 25(OH)D levels after adjusting them by gender (p = 0.024). In addition, the two SNPs in the GC gene (rs4588 and rs2282679) were identified significantly associated with iPTH and creatinine serum levels. In the case of phosphorus, we observed an association with GC SNPs in dominant model. We found a relationship between haplotype 2 and 25(OH)D levels, haplotype 4 and iPTH serum levels and haplotype 7 and phosphorus levels. In conclusion, genetic variants in CYP2R1 and GC could be predictive of 25(OH)D and iPTH serum levels, respectively, in older Caucasian adults. The current study confirmed the role of iPTH as one of the most sensitive biomarkers of vitamin D activity in vivo.     

鲜姜黄挥发油化学成分的GC-MS分析

目的:分析广西产鲜姜黄挥发油的化学成分,为其利用提供科学依据。方法:采用水蒸气蒸馏法提取鲜姜黄挥发油,用GC毛细管柱进行分析,归一化法测定其相对含量,并用GC-MS法鉴定化学成分。结果:检出48个色谱峰,鉴定出48个化合物,占总挥发油的100%。结论:广西产鲜姜黄油的的主要成分是姜烯(16.25%),1,8-桉叶油素(13.52%),芳-姜黄酮(13.55%),姜黄酮(11.19%),β-倍半水芹烯(10.08%),表-α-绿叶烯(6.26%),芳-姜黄烯(5.43%),大根香叶酮(5.02%),γ-松油烯(2.38%),红没药醇(3.59%)。