GC法测定醋氯芬酸含量

目的建立气相色谱法测定醋氯芬酸原料的含量的方法。方法气相色谱内标法。色谱柱为DB-1弹性毛细管柱(30 m×0.53 mm,1.5μm),FID检测器;汽化室温度为260℃,检测器温度300℃;柱温采用程序升温,载气为氮气,流速为5.0 mL.min-1,尾吹30 mL.min-1,分流比10∶1.以咖啡因为内标物。结果醋氯芬酸在10～110μg.mL-1(r=0.9998)范围内呈良好线性关系,平均回收率为100.1%。结论本方法简便,快速,准确,可靠,可用于醋氯芬酸的含量测定。     

丙泊酚的GC法测定

采用GC法测定丙泊酚的含量,以聚乙二醇丁二酸酯为固定液,2.1m×3.2mm的玻璃柱,柱温165°C.浓度在0.1～1.0mg/ml范围内,丙泊酚与内标物的峰面积的比值y与进样量x呈线性关系,y=2.66x-0.002(r=0.9998),RSD为0.18%.方法简便,结果可靠.     

“神奇戒烟灵”中吡啶的GC，GC／MS测定

利用气相色谱直接进样及气相色谱／质谱联机分析技术对戒烟灵中的吡啶进行了检测，并用外标法测定了吡啶的含量，方法简单、方便，结果准确、可靠。     

Phytotherapeutic activity of curcumol: Isolation,GC–MS identification,and assessing potentials against acute and subchronic hyperglycemia,tactile allodynia,and hyperalgesia

Context: Curcumol has recently attracted special attention due to its potential activities in many chronic disorders. Moreover, the traditional role of turmeric [Curcuma longa L. (Zingiberaceae)] in suppression of hyperglycemia is of great interest.

Objectives: The present work explores the potential acute and subchronic antihyperglycemic, antinociceptive, and in vivo antioxidant effects of curcumol in alloxan-diabetic mice.

Materials and methods: Bio-guided fractionation, column-chromatography, and GC–MS were utilized to identify the most active compound of turmeric (curcumol). Turmeric (25, 50, and 100?mg/kg), the curcumol rich fraction (CRF) (7?mg/kg), and curcumol (20, 30, and 40?mg/kg) were assessed for their acute (6 h) and subchronic (8 d) antihyperglycemic potentials and antinociceptive effects (8 weeks) were measured, using hot-plate and tail-flick latencies and von-Frey filaments method and in vivo antioxidant effects in alloxan-diabetic mice.

Results: The most-active turmeric fraction was found to be rich in curcumol (45.5%) using GC–MS analysis method. The results proved that the highest dose levels of turmeric extract and curcumol exerted remarkable hypoglycemic activity with 41.4 and 39.3% drop in the mice glucose levels after 6 h, respectively. Curcumol (40?mg/kg) was found to be 9.4% more potent than turmeric extract (100?mg/kg) in subchronic management of diabetes. Curcumol also showed a significant improvement of peripheral nerve function as observed from the latency and tactile tests.

Discussion: The antioxidant potential of curcumol may cause its ability to ameliorate diabetes and diabetes-related complications.

Conclusions: Curcumol, a natural metabolite with a good safety-profile, showed results comparable with tramadol in reversing diabetes-induced tactile allodynia and hyperalgesia.     

Characterization of identity, metabolism and androgenic activity of 17-hydroxyandrosta-3,5-diene by GC–MS and a yeast transactivation system

Anabolic–androgenic steroids are frequently misused compounds in sports, and they belong to the controlled substances according to the requirements of the World Anti-Doping Agency. The classical techniques of steroid detection are mass spectrometry coupled to gas or liquid chromatography. Biological methods that base on the ability of substances to bind the steroid receptor are not applied in routine doping control procedures so far, but they appear to be useful for characterization of steroid androgenic potential. In this study we used the yeast androgen receptor reporter system (YAS), which in the past has already successfully been applied to both various androgenic substances and also urine samples. Giving attention to the androgenic potential of steroidal dietary supplements, we exemplified the analysis using both mass spectrometry techniques and the YAS-based assay on the product “Syntrax Tetrabol” which was a confiscated dietary supplement and marketed as a steroid precursor. Identification, structure and the kinetic behavior of its excreted metabolites were analyzed by NMR, GC–MS and LC–MS/MS. The androgenic potential of the parent compound as well as its metabolites in urine was evaluated with the help of the YAS. The application of urine samples with a previous deconjugation and the inclusion of urine density values were carried out and led to increased responses on the YAS. Further, the possibility of a complementary application of structure-based instrumental analysis and biological detection of androgenicity with the help of the YAS seems to be desirable and is discussed.     

SPE结合GC—TID和GC—MS分析血浆中氨基甲酸酯类杀虫剂

目的：建立血浆中氨基甲酸酯类杀剂ＳＰＥ结合ＧＣ－ＦＩＤ和ＧＣ－ＭＳ的系统分析方法。方法：用ＳＰＥＣ Ｍｕｌｔｉ－Ｍｏｄａｌ混合相固相萃取柱建立血浆中５种氨基甲酸酯类杀虫剂的固相萃取方法;采用ＧＣ－ＭＳ作为定性分析工具,将保留时间、特征离子和谱库检索相结合实行多指标定性。结果：５种杀虫剂的绝对回收率在６０％～９６％之间,相对标准偏差小于９％（ｎ＝５）。结论：方法系统性好、快速、准确。     

GC测定醋酸中的乙醛残留量

目的 建立药用辅料醋酸中残留乙醛的测定方法。方法 醋酸用水稀释一倍后用等量的碱中和为盐溶液,立即密封后,采用顶空气相色谱法测定,以HP-INNOWAX石英毛细管柱(30 m×0.32 mm,0.5 μm)为分析柱,FID检测器;程序升温：35 ℃维持5 min,然后以30 ℃·min^-1升温至120 ℃,保持2 min;N₂流速为3.0 mL·min^-1;顶空进样：80 ℃平衡30 min。结果 醋酸的稀释避免了大量放热对测定的影响,中和生成的盐溶液提高了方法检测灵敏度,乙醛在10.73~ 107.3 mg·mL^-1(r=0.999 8)内线性关系良好,方法回收率为95.8％(n=9,RSD=5.0％),最低检出限为2.5 mg。结论 用简单的顶空气相色谱法,解决了醋酸中痕量乙醛残留的测定问题,为其国家标准的修订奠定了基础。     

用HPLC法和GC法测定

cicloprolol是一种β_1-肾上腺素能受体拈抗剂。本文报道了用HPLC法和GC法测定cicloprolol的血药浓度。贮备液的制备:精密称取cicloprolol和内标物倍他索洛尔的盐酸盐,分别溶于甲醇     

野菊花注射液的GC指纹图谱

目的建立野菊花注射液GC指纹图谱。方法使用DB-17弹性石英毛细管柱(30 m×0.25 mm,0.25μm)。柱温:初温80℃保持5 min,以5℃.min-1升至100℃保持10 min,5℃.min-1升至170℃保持5 min,10℃.min-1升至250℃保持3 min;载气:高纯氮气,流量,1.0 mL.min-1;分流比10∶1;氢气:40 mL.min-1;空气:400 mL.min-1;检测器:FID;检测器温度:280℃;气化室温度:280℃;进样量:1μL。结果建立了野菊花注射液的对照指纹图谱并确定了22个共有峰,各批注射液与对照指纹图谱相似度均在0.95以上。结论该方法简便、准确、重现性好,为野菊花注射液的质量控制提供了依据。     

白芷挥发油GC指纹图谱研究

目的:建立白芷挥发油成分的 GC 指纹图谱。方法:SE-30毛细管气相色谱柱(30 m×0.25 mm×0.25 μm),FID 检测器,程序升温为70℃(5 min),以2℃·min~(-1)的速度线性升温至220℃(5 min)。结果:依据21批药材的指纹图谱数据进行聚类分析,将样品分为4类,选定其中10批优质样品建立共有模式。相似度分析结果表明,第Ⅰ类和第Ⅱ类样品为优质药材,第Ⅲ类样品质量一般,第Ⅳ类样品为伪品。结论:本测定方法为白芷药材的质量评价提供了科学依据。     

辛夷挥发油的GC指纹图谱

目的建立辛夷挥发油指纹图谱测定方法,为辛夷药材的质量控制提供可靠方法。方法采用水蒸气蒸馏法提取不同产地的辛夷的挥发油;用毛细管气相色谱技术测定指纹图谱。色谱条件:DB-17石英毛细管色谱柱(30 m×0.25 mm,0.25μm,美国Agilent公司);氢火焰离子化检测器;进样口温度为250℃;检测器温度为250℃;柱温以65℃为起始温度,以2℃.min-1升温至90℃,以8℃.min-1升温至145℃,以2℃.min-1升温至155℃,以10℃.min-1升温至250℃,保持5 min。载气为氮气,流速为1.0 mL.min-1,分流比为5∶1,进样量为1μL。结果建立了辛夷药材的GC指纹图谱,标定了23个共有峰。结论该方法可为更好的控制辛夷药材的内在质量提供科学依据。     

薄荷素油的GC指纹图谱

目的：建立薄荷素油的GC指纹图谱。方法：采用弹性石英毛细管柱HP—FFAP（25m×0．20mm×0．33μm）;进样口温度250℃;Fid检测器检测器温度300％;载气为氮气;流速1．0ml·min^-1;分流比10：1;进样量1μl;程序升温：初始柱温65％,以5℃·min^-1升至100℃,再以2℃·min^-1升至200℃,总时间57min。结果：薄荷素油的GC指纹图谱由14个共有峰构成,所建立的指纹图谱具有稳定、重复性好的特点。结论：方法准确、简单,适用于薄荷素油的质量控制。     

小茴香挥发油GC指纹图谱研究

目的建立小茴香挥发油的GC指纹图谱,为其质量控制提供参考,同时也为中药标准指纹图谱库的建立奠定基础。方法利用水蒸气蒸馏法提取小茴香挥发油,并通过气相色谱法建立小茴香挥发油的特征指纹图谱。结果样品稳定性、仪器精密度和方法重现性良好,在此基础上建立了小茴香挥发油的特征指纹图谱。结论所得10批次小茴香挥发油的相似度都在0.90以上,符合国家药品监督管理局对中药指纹图谱的要求。     

GC测定硫唑嘌呤中吡啶残留量

目的建立气相色谱法测定硫唑嘌呤吡啶残留量方法。方法气相色谱法;检测器为FID;分流比为1∶30;进样口温度为140℃。结果平均回收率为102.8%,线性回归的相关系数r为0.999 7。结论气相色谱法能有效控制硫唑嘌呤中吡啶残留量。     

GC法测定丙酮酸乙酯的含量

摘 要 目的：建立测定丙酮酸乙酯原料含量的气相色谱法。方法: 色谱柱：Varian CP7502毛细管柱（25 m×0.25 mm,0.25 μm）;载气：氮气,流量为30 ml·min^-1;燃气：氢气,流量为40 ml·min^-1;助燃气：空气,流量为400 ml·min^-1;检测器：氢火焰离子化检测器（FID）;进样口温度：210 ℃;升温程序：初始温度为 40 ℃,以 15 ℃·min^-1的速度升至200 ℃;分流比：100∶1;进样量：1 μl。结果: 丙酮酸乙酯进样浓度在0.025 6~8.192 8 mg·mL^-1范围内与内标物的峰面积比值呈良好的线性关系（r=0.999 8）,平均加样回收率为99.99%,RSD为1.38%（n=9）。结论:建立的GC法准确、简便、快速、稳定性好,检测灵敏度高,适用于丙酮酸乙酯原料药的含量测定。     

GC法测定茴拉西坦含量

目的建立气相色谱法测定茴拉西坦含量的方法。方法气相色谱内标法。色谱柱为DB-1弹性毛细管柱,FID检测器;汽化室温度为260℃,检测器温度300℃;柱温200℃,载气为氮气,流速为5.0mL·min-1,尾吹50 mL·min-1,分流比10∶1,以咖啡因为内标物。结果茴拉西坦在10～110μg·mL-1(r=0.9998)范围内呈良好线性关系,平均回收率为100.1%。结论本方法简便,快速,准确,可靠,可用于茴拉西坦的含量测定。