气相色谱法测定发酵液中胆固醇的含量

气相色谱法测定了发酵液中胆固醇的含量。采用Rtx-1（100%二甲基聚硅氧烷）毛细管色谱柱、FID检测器进行分析测定。当胆固醇浓度在0～200μg/mL范围内与色谱峰面积呈良好线性关系（r=0.9981）。方法的平均回收率为99.38%,相对标准偏差为0.75%（n=8）,最低检出限可达到0.816μg/mL。气相色谱法作为发酵液中胆固醇含量的快速测定方法,具有试剂用量少、操作简单、结果准确等特点。     

气相色谱法测定生物制品中苯酚含量

本文采用气相色谱法测定了几种生物制品中苯酚含量。样品无需进一步处理,加入内标液后直接上柱测定,色谱峰形良好,线性范围宽,平均回收率和变异系数分别为１０１．８％ 和１．０８５％ ,最小检测限为１０ μｇ／ｍ ｌ,本法操作简单,样品用量少,可作为测定生物制品中苯酚含量的一种常规方法。     

气相色谱法测定紫杉醇注射液中乙醇的含量

目的:建立紫杉醇注射液中乙醇含量的测试方法。方法:采用氢火焰离子化检测器(FID)、以水为溶剂,采用DB-WAX聚乙二醇毛细管柱(30m×0.25mm×0.25um),载气为高纯氦,分流比79:1,柱温:80℃,检测器温度220℃,气化室温度220℃。结果:乙醇在1.03ug/ml-20.58ug/ml的范围内呈良好的线性关系,(r=0.9997),回收率为99.50%(RSD=0.56%),最低检测限为1.0ug/ml。结论:该方法简便、快速,满足于质量控制要求。     

高效液相色谱法测定丙谷胺片的含量

丙谷胺是一种胃泌素拮抗剂,其含量测定方法《中国药典》2000年版二部及《中国药典》2005年版二部采用的是滴定法,本文试用高效液相色谱法（HPLC法）测定其含量,此法操作简便,重现性好,结果准确可靠。     

高效液相色谱法测定西咪替丁片的含量

目的建立HPLC测定西咪替丁片含量的方法。方法固定相:sinochrom ODS-BP 5μm(4.6 mm×250 mm);流动相:甲醇∶水∶三乙胺(80∶20∶0.01),流量为1.0 ml/min;检测波长:218nm,进样量10μl。结果对照品溶液在0.25~2.0μg/ml范围内呈良好的线性关系,相关系数r=0.9996(n=6),平均回收率为99.23%(n=6),RSD为0.4%。结论本法快速、简便、准确、重复性好。     

丹葛酚酮胶囊HPLC指纹图谱及9种有效成分的含量测定

建立丹葛酚酮胶囊的HPLC指纹图谱,并同时测定其中9种有效成分的含量,为其质量评价提供依据。采用Eclipse XDB-C₁₈色谱柱(4.6 mm×250 mm,5μm),以0.05%甲酸-乙腈为流动相梯度洗脱,流速1.0 mL/min,检测波长280 nm,柱温30℃,进样量10μL,建立了丹葛酚酮胶囊的HPLC指纹图谱。10批丹葛酚酮胶囊指纹图谱中有28个共有峰,相似度均大于0.99,经与对照品比对确认了16个成分,对葛根素、3′-羟基葛根素、3′-甲氧基葛根素、葛根素芹菜糖苷、大豆苷、丹酚酸B、隐丹参酮、丹参酮Ⅰ、丹参酮Ⅱ_A 9种主要成分进行了定量分析,线性、精密度、稳定性、重复性和加样回收率均符合定量要求,所建立的方法简便、稳定、可靠,指纹图谱结合多指标成分的含量可有效控制产品的质量。     

气相色谱法测定食品中植物甾醇含量研究

目的：建立气相色谱法测定食品中植物甾醇含量的方法。方法：对常见食品中的菜油甾醇、豆甾醇、β-谷甾醇含量进行定性定量分析。食品样品经皂化后提取,浓缩后用正己烷定容,上机测定。结果：本方法可有效分离食品中植物甾醇组分,各组分在0.005~0.2 mg/mL范围内线性关系良好,相关系数R2均在0.99以上;检出限为0.3 mg/100 g,其回收率在84.9%~106.2%,方法的重现性、精密度和稳定性良好,RSD均小于5%。结论：与液相色谱法相比,本方法能够有效分离和测定植物甾醇组分,且具有样品前处理简单、方法重现性好、准确度和灵敏度高等优点,可用于测定食品中植物甾醇组分含量。     

顶空毛细管气相色谱法测定阿魏酸钠中有机溶剂残留量

建立了顶空毛细管气相色谱法测定阿魏酸钠中的乙醇、哌啶与吡啶。采用DB-624毛细管色谱柱,FID检测器,程序升温。3种溶剂在一定浓度范围内线性关系良好,平均回收率分别为99.3%、100.1%和99.5%,RSD均小于1.0%。     

高效液相色谱法测定山栀子中栀子甙的含量

采用高效液相色谱法测定中药山栀子（Cardenia jasminoides Ellis）中保肝利胆的主要成分栀子甙（geniposide）的含量。分析结果表明,本方法重现性好,平均加样回收率为100．90％,RSD为2．00％。用此方法测定未知样品山栀子中栀子甙的平均含量为3．463g/100g。     

气相色谱法测定抗毒素中的间甲酚含量

采用气相色谱法测定抗毒素中的间甲酚含量。样品用苯甲醇作内标,经高氯酸沉淀蛋白、氯仿抽提后,通过HP-INNO-WAX柱,以氢火焰检测器测定间甲酚含量。内标峰与样品峰的分离度大于1.5,平均回收率及变异系数分别为100.067%和1.93%,测定线性范围0.0202~1.7588mg/ml,最小检测限为0.01272mg/ml,该方法准确快速,比化学方法好。     

速效止泻胶囊含量测定方法的初步研究

目的：探讨速效止泻胶囊质量标准中含量测定方法的建立。方法：采用中性氧化铝柱层析-紫外分光光度法建立了盐酸小檗碱的含量测定方法。结果：线性关系r=0.99996,平均回收率为106．42％,含量限度为90mg/粒。结论：建立的含量测定方法准确可靠,可以控制产品质量。     

Identification and Determination of Tele-Methylhistamine in Cerebrospinal Fluid by Gas Chromatography-Mass Spectrometry

Abstract: The presence of tele-methylhistamine in human cerebrospinal fluid has been established. The concentration was determined with the use of deuterated tele-methylhistamine. The preparation of the deuterated standard is described. The concentration range in samples from neuropsychiatric patients was 0.1-2.5 ng/ml. The structure of the pentafluoropropionyl derivative used for gas chromatography was studied with the aid of proton nuclear magnetic resonance spectroscopy.     

毛细管气相色谱内标法测定核桃油中的脂肪酸

测定了核桃油的脂肪酸组成,建立了以十七烷酸甲酯为内标物,用毛细管气相色谱同时测定核桃油五种脂肪酸（棕榈酸、硬脂酸、油酸、亚油酸、亚麻酸）的方法。样品经氢氧化钾．甲醇皂化、三氟化硼．甲醇酯化后使生成相应的脂肪酸甲酯,以DM-FFAP毛细管柱分离,火焰离子化检测器测定。用保留时间定性,内标法定量。结果表明,在所选择的条件下,核桃油脂肪酸在10min内能获得较好的分离;五种脂肪酸的峰面积与其质量浓度有良好的线性关系,相关系数均大于0．998;样品加标回收率（n=6）为92．5％-100．3％,相对标准偏差为2．41％-4．31％。该方法操作简便、快速、准确,适合批量样品的测定。     

用HPLC法测定发酵液中的生物素含量

采用高效液相色谱法测定发酵液中生物素的含量。色谱柱为Symmetry C18,流动相为V(甲醇):V(pH 2.5磷酸缓冲溶液)=14:86,检测波长为210 nm,柱温为35℃。结果表明,样品进样量在5-150μg/mL范围内线性关系良好,加样回收率在95%以上,相对标准偏差RSD为6.6%,最低检测限为0.01μg/mL。该方法简便、快捷、准确、重现性好,可用于发酵液中生物素的含量测定。     

高效液相色谱法同时检测棉花根中的多种植物激素

目的：探寻高效液相色谱同时检测棉花根中多种植物激素含量的方法。方法：采用WatersC18反相色谱柱（4.6×250mm,5μm）,在柱温为35℃、流速为1mL.min-1的条件下,以乙腈和三乙胺溶液为流动相梯度洗脱,在每种物质的保留时间附近切换至最大吸收峰（GA3除外）波长作为检测波长,并与254nm同一波长检测多种植物激素含量的方法进行比较,分离和检测棉花根中的玉米素（Z）、玉米素核苷（ZR）、赤霉酸（GA3）、生长素（IAA）和脱落酸（ABA）的含量。结果：切换波长法检测5种植物激素的灵敏度和回收率均较高,检出限均较低。回收率为：Z 96.82%、ZR 94.14%、GA3 92.75%、IAA 93.38%、ABA 95.57%;检出限为：Z 0.1μg.mL-1、ZR 0.1μg.mL-1、GA3 0.5μg.mL-1、IAA 0.3μg.mL-1;ABA 0.05μg.mL-1,能准确检测出棉花根中Z、ZR、GA3、IAA和ABA的含量。结论：采用Waters C18反相色谱柱（4.6×250mm,5μm）,在柱温为35℃、流速为1mL.min-1的条件下,以乙腈和三乙胺溶液为流动相梯度洗脱,结合切换波长法能同时检测出植物组织中多种植物激素含量。     

拟南芥中4种细胞分裂素的高效液相色谱法测定

应用高效液相色谱法同时测定拟南芥中4种细胞分裂素组分玉米素(Z)、玉米素核苷(ZR)、6-r,r-二甲基烯丙基氨基嘌呤(2ip)和6-r,r-二甲基烯丙基氨基嘌呤核苷(2ipr)含量。结果表明,采用反相色谱柱Waters C₁₈柱(4.6×250 mm,5 μm),在35℃以乙腈和三乙胺缓冲液为流动相梯度洗脱,流速1 ml/min,在270 nm处能准确检测出拟南芥中4种细胞分裂素组分的含量,检测限达0.001 μg/ml。     

Simultaneous quantification of jasmonic acid and salicylic acid in plants by vapor-phase extraction and gas chromatography-chemical ionization-mass spectrometry

Jasmonic acid and salicylic acid represent important signaling compounds in plant defensive responses against other organisms. Here, we present a new method for the easy, sensitive, and reproducible quantification of both compounds by vapor-phase extraction and gas chromatography-positive ion chemical ionization-mass spectrometry. The method is based on a one-step extraction, phase partitioning, methylation with HCl/methanol, and collection of methylated and, thus, volatilized compounds on Super Q filters, thereby omitting further purification steps. Eluted samples are analyzed and quantified by GC/MS with chemical ionization. Standard curves were linear over a range of 5-1000 ng for jasmonic acid and salicylic acid. The correlation coefficients were greater than 0.999 and the recovery rates estimated between 70 and 90% for salicylic acid and 90 and 100% for jasmonic acid. The limit of detection was about 500 fg by using single ion detection mode. Both, cis- and trans-isomers for jasmonic acid can be detected. A comparison with established methods indicates the new method to be highly efficient, allowing reliable quantification of both compounds from small amounts of plant material (5-400mg fresh weight).     

Determination of aldehydes in exhaled breath of patients with lung cancer by means of on-fiber-derivatisation SPME–GC/MS

A number of volatile organic compounds (VOCs) have been identified and used in preliminary clinical studies of the early diagnosis of lung cancer. The aim of this study was to evaluate the potential of aldehydes (known biomarkers of oxidative stress) in the diagnosis of patients with non-small cell lung cancer (NSCLC). We used an on-fiber-derivatisation SPME sampling technique coupled with GC/MS analysis to measure straight aldehydes C3–C9 in exhaled breath. Linearity was established over two orders of magnitude (range: 3.3–333.3 × 10⁻¹² M); the LOD and LOQ of all the aldehydes were respectively 1 × 10⁻¹² M and 3 × 10⁻¹² M. Accuracy was within 93% and precision calculated as % RSD was 7.2–15.1%. Aldehyde stability in a Bio-VOC^® tube stored at +4 °C was 10–17 h, but this became >10 days using a specific fiber storage device. Finally, exhaled aldehydes were measured in 38 asymptomatic non-smokers (controls) and 40 NSCLC patients. The levels of all of the aldehydes were increased in the NSCLC patients without any significant effect of smoking habits and little effect of age. The good discriminant power of the aldehyde pattern (90%) was confirmed by multivariate analysis. These results show that straight aldehydes may be promising biomarkers associated with NSCLC, and increase the sensitivity and specificity of previously identified VOC patterns.     

Determination of malondialdehyde in biological fluids by high-performance liquid chromatography using rhodamine B hydrazide as the derivatization reagent

Malondialdehyde (MDA) is a biomarker for lipid peroxidation, and studies of sensitive and selective analytical methods for it are very important for pathological research. The aim of this work was to develop and validate a novel HPLC method for the quantification of MDA in biological fluids using rhodamine B hydrazide (RBH) as the derivatization reagent. After pretreatment and derivatization in acid medium at 50 °C for 40 min, the RBH-derivatized MDA was separated on a Kromasil C₁₈ column at 25 °C and detected by a fluorescence detector at excitation wavelength of 560 nm and emission wavelength of 580 nm. The results showed linearity in the range of 0.8–1500.0 nM with a detection limit of 0.25 nM (S/N = 3). The recovery of MDA from plasma and urine was 91.50 to 99.20%, with a relative standard deviation range of 1.45 to 3.26%. In comparison to other methods reported for the determination of MDA, the proposed method showed superiority in simplicity, more sensitivity, shorter derivatization time, and less interference. The developed method was applied to quantification of MDA in human biological fluids collected from five volunteers with a concentration range of 24.62–245.00 nM.