HPLC法测定复方金沙利胆颗粒中芍药苷的含量

目的建立复方金沙利胆颗粒中芍药苷的含量测定方法及质量控制研究。方法色谱柱为We Lch Utimate XB-C₁₈（4.6 mm×250 mm,5μm）,流动相:乙腈-纯水（17∶83）,流速1.0 m L·min^-1,柱温室温,检测波长230 nm,进样量20μL。用高效液相色谱法对芍药苷进行定量测定;对主要成分黄芩、白芍、枳壳等进行薄层鉴别。结果用该方法定性鉴别专属性强,芍药苷在浓度3.92⁹8μg·m L^-1内呈现良好的线性关系（r=0.9995）。芍药苷平均回收率为98.11%,RSD为1.10%（n=6）。结论该方法简便,准确,重现性好,分离度好,回收率高,能有效对复方金沙利胆颗粒的质量进行控制和评价。     

HPLC法同时测定化痔胶囊中柚皮苷、新橙皮苷的含量

目的:建立化痔胶囊中柚皮苷、新橙皮苷的高效液相色谱法(HPLC)含量测定方法。方法:以乙腈-0.5%磷酸(42∶58)为流动相,检测波长为283 nm,采用HPLC对化痔胶囊中柚皮苷、新橙皮苷的进行含量测定。结果:柚皮苷和新橙皮苷分别在0.4658~9.3160μg(r=0.9997)、0.2834~5.6680μg(r=0.9994),进样量与峰面积呈良好的线性关系,平均加样回收率分别为99.89%、99.07%,RSD(n=6)分别为1.32%、1.85%。结论:方法简便、准确、灵敏、重复性好,可作为化痔胶囊中的柚皮苷和新橙皮苷含量控制方法。     

高效液相色谱法测定复方柴黄软胶囊中黄芩苷含量

目的:建立高效液相色谱法(HPLC)测定清热丸中黄芩苷的含量.方法:采用反相高效液相色谱法,色谱柱为十八烷基硅烷键合硅胶(4.6 mm×250 mm,5μm);流动相:甲醇-水-磷酸(50:50:0.2);检测波长:280 nm;流速为1.0 ml/min;柱温为40℃.结果:黄芩苷线性范围为0.4-2.0μg,r=0.9998,平均回收率=98.90%,黄芩苷RSD=1.3%(n=6).结论:方法简便、准确、重现性好,可作为该制剂的含量测定方法.     

高效液相色谱法测定元神安颗粒中芍药苷的含量

目的：建立元神安颗粒中芍药苷的含量测定方法.方法：高效液相色谱法测定赤芍的主要有效成分芍药苷的含量.色谱柱为Diamonsil C18柱（250mm×4.6mm,5μm）,流动相为乙腈-水（15：85）,检测波长为230nm.结果：芍药苷在0.2116-3.174μg范围内线性关系良好（r=0.9996）,加样回收率99.7%,RSD=1.3%（n=6）.结论：该法简便、准确、重现性好.     

HPLC法测定小儿风热清颗粒中栀子苷的含量

应用高效液相色谱法测定小儿风热清颗粒(XEFRQKL)中栀子苷的含量.方法:采用C18色谱柱(4.6mm×250mm,5μm),乙腈-0.5%磷酸溶液(10:90)为流动相,流速为1.0ml/min,检测波长为238nm.结果表明,栀子苷在0.07392～0.44352ug范围内,进样量与峰面积呈良好的线性关系(r=0.9999),平均加样回收率为98.82%,RSD=1.58%(n=5).该方法测定结果准确、灵敏、重复性好.     

HPLC法测定众生片中黄芩苷的含量

目的:采用高效液相法测定众生片中黄芩苷的含量。方法:色谱柱为HypersilC18(4.6mm×200mm,5μm;流动相为甲醇-水-磷酸(45:55:0.2);流速为:1ml.min-1;检测波长为278nm.。结果:黄芩苷进样量在0.0150.15ug之间,与峰面积呈良好的线性关系(r=0.9999),平均加样回收率为96.57%,RSD=1.3%(n=5)。结论:本方法操作简单,快捷,可用于测定众生片中黄芩苷的含量。     

赤芍中芍药苷的超声波强化醇提工艺优化

采用超声波强化过程提取技术,以乙醇为萃取溶剂提取芍药苷,用高效液相色谱(HPLC)分析检测方法分析芍药苷浓度,并以芍药苷提取得率为评价标准。通过正交设计方法,选择乙醇与药材之间的倍量、提取时间、提取次数、乙醇浓度四因素进行正交试验,优化超声波法醇提赤芍中芍药苷的工艺条件。通过残差分析和方差分析,确定赤芍超声提取的最佳工艺条件为:6倍量的70%乙醇溶液,超声提取3次,每次1 h,提取次数对芍药苷的含量影响最大。在优化实验条件下,从赤药中提取的芍药苷含量为36.04 mg/g。     

气滞胃痛颗粒中橙皮苷、柚皮苷含量的测定

目的:建立反相高效液相色谱法测定气滞胃痛颗粒中柚皮苷和橙皮苷的方法.方法:采用SHIMAD-ZU VP-ODS(4.6mm×150mm,5μm)色谱柱;乙腈-pH3.5磷酸水=22:78(v/v)为流动相,流速为1.2 ml·min-1;检测波长为283nm.结果:待测组分与其他组分分离度良好(>1.5),柚皮苷和橙皮苷线性范围分别为2.8-56.0μg·ml-1和0.43-8.6μg·ml-1,柚皮苷和橙皮苷的平均回收率分别为98.9%,99.6%,RSD分别为1.7%,2.0%.结论:本方法简便,准确度和精密度均能满足橙汁饮料中橙皮苷、柚皮苷测定的要求.     

HPLC法同时测定热淋清胶囊中没食子酸、原儿茶酸、槲皮苷和槲皮素的含量

建立热淋清胶囊中没食子酸、原儿茶酸、槲皮苷和槲皮素的HPLC定量方法.采用Wa-ters色谱柱,乙腈-0.4%磷酸为流动相梯度洗脱,流速1.0 mL/min,检测波长254 nm,柱温40℃.没食子酸、原儿茶酸、槲皮苷和槲皮素的线性范围分别为1.376~9.632μg,0.041 6~0.291 2μg,0.061 5~0.430 5μg,0.006 702~0.046 914μg;平均回收率分别为98.71%(RSD=1.17%)、98.77%(RSD=1.92%)、99.19%(RSD=1.92%)、100.39%(RSD=1.99%).所建立的方法准确、稳定,重现性好,可用于热淋清胶囊中有效成分的定量分析.     

HPLC测定利胆消炎颗粒中黄芩苷的含量

目的:采用高效液相色谱法测定利胆消炎颗粒中黄芩苷的含量.方法:色谱柱为Waters C18柱,流动相为甲醇-0.2%磷酸溶液(47:53),检测波长为280nm,流速为1.0mL/min.结果:黄芩苷进样量线性范围是10.0μg/mL～100μg/mL(r=0.9999),平均加样回收率98.80%,RSD=1.70%(n=6).结论:该方法简便、灵敏,可用于制剂的质量控制.     

RP—HPLC法测定乳酸左氧氟沙星含量

目的：建立乳酸左氧氟沙星氯化钠注射液中主药的含量测定方法。方法：采用反相高效液相色谱法。以Lichrospher5-C18为色谱柱;己烷磺酸钠-甲醇（3：1）为流动相;流速为1．0ml／min;检测波长为293nm,柱温为40℃,进样量为20u1。结果：乳酸左氧氟沙星浓度在5．0-50．0μg／ml内线性关系良好（r=0．9995）,平均回收率为99．85％。RSD为0．25％。结论：此法准确可靠,重现性好,能有效控制乳酸左氧氟沙星氯化钠注射液的质量。     

桑姜感冒胶囊中总黄酮含量的测定

目的：建立桑姜感冒胶囊中总黄酮含量的测定方法。方法：采用紫外-可见分光光度法,以芦丁为对照品,以506 nm作为测量波长进行测定。结果：芦丁在0.5~3.0 mg范围内与吸光度呈良好的线性关系（r=0.999 7）,平均回收率为96.63%,RSD为1.91%。结论：该方法操作简便、准确、重现性好,可用于测定桑姜感冒胶囊中总黄酮的含量。     

Effect of small bowel preparation with simethicone on capsule endoscopy

Background: Capsule endoscopy is a novel non-invasive method for visualization of the entire small bowel. The diagnostic yield of capsule endoscopy depends on the quality of visualization of the small bowel mucosa and its complete passage through the small bowel. To date, there is no standardized protocol for bowel preparation before capsule endoscopy. The addition ofsimethicone in the bowel preparation for the purpose of reducing air bubbles in the intestinal lumen had only been studied by a few investigators. Methods: Sixty-four participants were randomly divided into two groups to receive a bowel preparation of polyethylene glycol (PEG) solution (Group 1) and both PEG solution and simethicone (Group 2). The PEG solution and sime-thicone were taken the night before and 20 min prior to capsule endoscopy, respectively. Frames taken in the small intestine were examined and scored for luminal bubbles by two professional capsule endoscopists. Gastric emptying time and small bowel transit time were also recorded. Results: Simethicone significantly reduced luminal bubbles both in the proximal and distal small intes-tines. The mean time proportions with slight bubbles in the proximal and distal intestines in Group 2 were 97.1% and 99.0%, respectively, compared with 67.2% (P<0.001) and 68.8% (P<0.001) in Group 1. Simethicone had no effect on mean gastric emptying time, 32.08 min in Group 2 compared with 30.88 min in Group 1 (P=0.868), but it did increase mean small intestinal transit time from 227.28 to 281.84 min (P=0.003). Conclusion: Bowel preparation with both PEG and simethicone significantly reduced bubbles in the intestinal lumen and improved the visualization of the small bowel by capsule endoscopy without any side effects observed.     

Application of derivative ratio spectrophotometry for determination of β-carotene and astaxanthin from Phaffia rhodozyma extract

INTRODUCTION Carotenoids are a class of natural fat-solublepigments generally found in plants, algae, and pho-tosynthetic bacteria, where they play a critical role inthe photosynthetic process. Carotenoids also exist insome non-photo-synthetic bacteria, yeasts, and moldswhere they may carry out a protective functionagainst damages by light and oxygen. Although ani-mals can not synthesize carotenoids within theirbodies, they can intake carotenoids from their dietsleading to bright meat col…     

高效液相色谱法测定宝宝乐颗粒中芍药苷的含量

目的：建立宝宝乐颗粒中芍药苷的高效液相色谱（HPLC）测定方法。方法：采用Diamonsil C18（4．6×250mm,5um）色谱柱,以乙腈-水-磷酸（20：80：0．05）为流动相,检测波长：230nm,流速：1．0mL/min,柱温：35．0℃。结果：芍药苷在0．1540ug～1．2320ug范围内与峰面积线性关系良好,相关系数为r=0．9999,平均回收率为99．82％（RSD=0．301％,n=5）。结论：HPLC法操作快速、简便、结果准确,可作为宝宝乐颗粒中芍药苷的定量分析方法。     

气相法测定氟马西尼中乙醇、乙醚、二氯甲烷残留量

建立顶空气相色谱法控制氟马西尼中有机溶剂乙醇、乙醚、二氯甲烷残留量的分析方法。方法：采用DB-624石英毛细管柱,FID离子化检测器,以90%的二甲亚砜水溶液为溶剂。结果：乙醇在12.60～75.60ug/ml（630ppm～3780ppm）的浓度范围内,r为0.9998乙醚在12.79～76.74ug/ml（639.5ppm～3837ppm）的浓度范围内,r为0.9999二氯甲烷在2.54～15.24ug/ml（127ppm～762ppm）的浓度范围内,r为0.9997,大于规定的0.99;定量限试验中,信噪比符合规定,能够达到定量检测及检出的要求;各浓度下的乙醇、乙醚、二氯甲烷平均回收率均在90%-110%范围内。结论：该方法专属性好,精密度、准确度都符合要求,方法可靠,可用于原料药氟马西尼中有机溶剂乙醇、乙醚、二氯甲烷的残留量的控制。     

高效液相色谱法测定小儿启脾颗粒的含量

目的:建立高效液相色谱法测定小儿启脾颗粒含量的方法。方法:采用Inertsil C18色谱柱,流动相为乙腈-0.05%磷酸溶液(20:80);流速:1.0ml·min^-1;检测波长为203nm。结果:线性范围为0.2024~1.6192μg·ml^-1(r=0.9998),样品平均加样回收率(n=6)为97.8%,RSD为0.46%。结论:本法结果准确,重现性好,可用于小儿启脾颗粒的质量控制。     

牛磺酸滴眼液中牛磺酸含量的测定

目的:测定牛磺酸滴眼液中牛磺酸的含量。方法:采用分光光度法测定牛磺酸滴眼液中牛磺酸的含量。结果:牛磺酸在10～60mg/ml浓度范围内呈良好的线性关系,回收率为99.3%(n=6)。结论:牛磺酸滴眼液中牛磺酸的平均为0.034mg/ml,方法稳定性良好,操作简单易行,符合药品定量分析要求。     

Hyperechoic demarcation line between a tumor and the muscularis propria layer as a marker for deciding the endoscopic treatment of gastric submucosal tumor

Minimally invasive endoscopic resection has been rapidly adopted as a new technique for treating patients with gastric submucosal tumors (SMTs) originating in the muscularis propria (MP) layer. This study was conducted to evaluate the information obtained from endoscopic ultrasonography (EUS) to determine the appropriate endoscopic dissection method for treating SMTs originating in the MP layer. Between February 2014 and May 2016, a total of 50 patients with gastric SMTs originating in the MP layer were enrolled in this study. The clinical features of the patients and their endoscopic, EUS, and histopathologic findings, as well as their postoperative follow-up data, were analyzed in this retrospective study. The mean age of the patients was (55.0±10.2) years, and the male/female ratio was 17:33. Endoscopic submucosal dissection (ESD) was performed on 43 patients and an endoscopic full-thickness resection (EFR) was performed on seven patients. The most frequent location for an SMT was in the upper body region of the stomach (n=16), and the most common pathological diagnosis was a gastrointestinal stromal tumor (GIST) (n=32). The overall rates for complete resection were 95.3% (41/43) and 100.0% (7/7) when the SMTs were treated by ESD and EFR, respectively. The presence of a complete tumor capsule was significantly associated with a complete resection (P=0.001). Of the cases treated by ESD, nine patients developed perforation, one of whom required laparoscopic surgery. The remaining patients were closed with clips or purse-string sutures. The presence of an MP2-type tumor (P=0.018) and a wide connection with the MP layer (P=0.044) were significantly associated with perforation. A preoperative evaluation of the integrity and the location of a tumor capsule and the length of the tumor connection with the MP layer by EUS can improve the complete resection rate and reduce the occurrence of intraoperative complications. Tumors with a complete capsule originating from the superficial MP layer or with a narrow connection with the MP layer are appropriate candidates for treatment by ESD.     

流动注射氢化物发生原子吸收光谱法测油酸钠中砷的含量

建立一种油酸钠中微量砷的测量方法。方法:用氢化物-原子吸收分光光度法,在砷的特征谱线193.70nm用标准加入法测定油酸钠中砷的含量。线性回归方程为C=43.9445A-1.0075,R=0.99908。线性范围为0.5-6ng·mL-1,检测限是0.309ng·mL-1,油酸钠的回收率为94.3%～105.2%,相对标准偏差为3.26%,结论:该法检测限低、灵敏度高,是一种非常有效的分析方法。