毛细管气相色谱法测定霉酚酸酯原料药中有机溶剂残留量

建立毛细管气相色谱法测定霉酚酸酯原材料药中5种有机溶剂残留量。采用DB–WAX弹性石英毛细管色谱柱(30 m×0.53 mm,0.5μm),氢火焰离子化检测器(FID),两次程序升温测定,5种有机溶剂能完全分离(R2.0)。乙酸乙酯、乙基苯、对二甲苯、间二甲苯、邻二甲苯的线性范围分别为5.120~512.0,2.010~201.0,2.110~211.0,2.000~200.0,2.080~208.0μg/mL(r0.999),检出限分别为1.710,0.960,1.000,0.95,0.990μg/mL,平均加标回收率为96.0%~103.0%,测定结果的相对标准偏差为0.76%~0.99%(n=9)。该方法准确,灵敏度高,可用于霉酚酸酯原料药中有机溶剂残留检测。     

毛细管气相色谱法测定鱼油食品中的脂肪酸DHA,EPA

采用毛细管气相色谱法测定鱼油中DHA和EPA的含量,色谱柱为DB–WAX型毛细管柱(30 m×0.530mm,1.00μm),柱温采用程序升温,载气为氮气,流速15 mL/min,FID检测器,温度为300℃,进样口温度260℃,分流比为10∶1,进样量为1μL。DHA及EPA的质量浓度(X)分别在0.25~20.0,0.125~10.0 mg/mL范围内与色谱峰面积(Y)呈良好的线性关系,线性方程分别为Y=905417X+6060.6,Y=887335X+4463.6,线性相关系数r均为0.9999,平均回收率分别为97.8%,96.1%,相对标准偏差小于3%(n=6)。该方法简便、重现性好,可用于鱼油中DHA和EPA含量测定。     

气相色谱法测定丙烯氧化生产丙烯酸尾气中丙烯醛、乙酸、丙烯酸含量

采用毛细管气相色谱法测定丙烯氧化生产丙烯酸尾气中丙烯醛、乙酸、丙烯酸的含量,色谱柱为FFAP(30m×0.53 mm,1μm),检测器为FID,用外标法进行定量,尾气样品中丙烯醛、乙酸、丙烯酸的检出限分别为0.025,0.033,0.031 mg/m3,测定结果的相对偏差为0.97%~2.63%(n=5),加标回收率为98.29%~103.60%。     

气相色谱法测定酚醛树脂中游离苯酚

建立气相色谱外标标准曲线法测定酚醛树脂中游离苯酚的含量。采用DB–5(30 m×0.25 mm, 0.25μm)色谱柱,程序升温,气化室温度为250℃,以火焰离子化检测器(FID)检测,检测器温度为280℃,以标准曲线外标法计算游离苯酚含量。苯酚的质量浓度在0.05～10.0 mg/mL范围内与色谱峰面积呈良好的线性关系,线性相关系数(r)为1,方法检出限为0.003 7 mg/mL。样品加标回收率为98.0%～102.0%,测定结果的相对标准偏差为1.07%～1.26%(n=6)。该方法简单、快速,测定结果准确、可靠,可用于酚醛树脂中游离苯酚含量的检测。     

双波长UPLC同时测定桃金娘根中没食子酸和鞣花酸

建立了超高效液相色谱(UPLC)结合二极管阵列检测器(PDA)同时测定桃金娘根中没食子酸和鞣花酸的方法。样品经过甲醇超声提取,过滤,蒸干甲醇,残渣用二甲基亚砜定容。采用Waters BEH C18色谱柱(2.1×100 mm1.7μm),以乙腈-0.2%H2PO4溶液为流动相进行梯度洗脱,流速0.25 m L/min,检测波长为271 nm和253 nm。没食子酸在0.686~68.600μg/m L,鞣花酸在0.504~50.373μg/m L浓度范围内呈良好线性关系,相关系数分别为0.9999,0.9999;样品加标平均回收率分别为97.2%~99.0%、96.2%~98.9%;没食子酸和鞣花酸峰面积的RSD分别为1.1%和1.9%,迁移时间RSD为0.9%和1.3%;检出限分别为0.45和0.23 ng/m L。     

顶空-气相色谱法测定葡萄糖氯化钠注射液中12种溶剂残留量

建立顶空-气相色谱法测定葡萄糖氯化钠注射液中12种残留溶剂含量的方法。采用HP-INNOWAX毛细管色谱柱(60 m×320μm,0.5μm)为分离柱,检测器为氢火焰离子化检测器(FID),柱温为程序升温。12种残留溶剂乙醇、异丙醇、丙酮、丁酮、乙酸乙酯、乙酸丁酯、乙酸正丙酯、甲苯、乙苯、对二甲苯、邻二甲苯、间二甲苯均能完全分离,在考察的浓度范围内线性关系良好(r>0.995),检出限分别为0.055,0.019,0.023,0.070,0.155,0.013,0.003,0.009,0.004,0.004,0.004,0.005μg/mL。平均回收率为90.6%~109.0%,测定结果的相对标准偏差为2.2%~5.6%(n=9)。该方法专属性强,精密度、准确度和检测灵敏度高,重复性好,可用于葡萄糖氯化钠注射液中12种溶剂残留量的测定。     

毛细管气相色谱法快速测定对氯甲苯及对氯苯甲醛

建立了在乙酸作为反应溶剂条件下空气催化氧化对氯甲苯反应液组分含量的快速分析方法,采用毛细管柱DB-FFAP(15 m×0.25 mm i.d.,0.25μm),检测器为FID氢火焰离子化检测器,以薄荷脑为内标对反应液进行气相色谱分析,采用程序升温,对氯甲苯及对氯苯甲醛在5.0 min内实现基线分离.该方法具有良好的重现性和线性关系,对氯甲苯及对氯苯甲醛回收率分别为:98.6%、101.7%,相对标准偏差分别为:0.30%、O.32%.该方法分析速度快,可用于对氯苯甲醛合成工艺优化和样品的质量控制以及生产过程中大量样品快速定量测定.     

复方丹参片中四种成分的高效液相色谱-电化学检测-紫外检测法分析

建立了电化学检测器与二极管阵列检测器联用的液相色谱(HPLC-ECD-DAD)同时分离和测定复方丹参片中原儿茶酸、原儿茶醛、咖啡酸和丹参酮ⅡA 等4种成分的分析方法。采用Zorbax SB-C18柱(150 mm×4.6 mm i.d.,5.0 μm),以甲醇和0.4%磷酸为流动相(流速1.0 mL/min)进行梯度洗脱;ECD检测电压0.7 V,DAD检测波长270 nm,柱温30 ℃。实验结果表明,原儿茶酸、原儿茶醛、咖啡酸和丹参酮ⅡA质量浓度分别为0.3～9.0 mg/L,1.1～54.0 mg/L,1.1～11.1 mg/L和5.2～52.0 mg/L时与其峰面积呈良好的线性关系(线性相关系数均高于0.999),原儿茶酸、原儿茶醛、咖啡酸和丹参酮ⅡA的平均回收率(n=6)分别为97.8%(相对标准偏差(RSD)为2.15%),98.2%(RSD为2.07%),97.6%(RSD为2.18%)和97.2%(RSD为2.07%)。该法同时利用了ECD和DAD的优点,是一种快速、灵敏、准确的分析方法,可以为复方丹参片的质量控制提供科学依据。     

气相色谱测定海绵文胸中甲苯二异氰酸酯残留

建立了气相色谱-内标法测定海绵文胸中的甲苯二异氰酸酯(TDI)残留量。样品经均质处理后,用经脱水处理的乙酸乙酯超声萃取25 min,过滤净化后,采用Agilent DB-624色谱柱(30 m×0.32 mm×1.8μm)分析,柱温采用程序升温,检测器为氢火焰离子化检测器,检测器温度为250℃,进样口温度为180℃,载气为氮气。结果表明:甲苯二异氰酸酯在10~200 mg/L范围内峰面积与质量浓度线性关系良好,线性相关系数(R~2)为0.998 9,平均回收率为80.5%~91.6%,RSD不大于7.9%(n=6),方法的检出限和定量限分别为10 mg/kg和100 mg/kg。在优化条件下,对生产企业、实体店和电商平台采购的100批次样品进行了检测。该方法操作简单、耗时短、灵敏度高、稳定性好,应用于日常检测可大大降低检测成本,缩短检测周期,具有实际应用价值。     

超高效液相色谱/质谱法测定血液中γ-氨基丁酸

研究了超高效液相色谱-质谱检测器(UPLC-QDa)对γ-氨基丁酸的分析检测,建立了UPLC测定血液中γ-氨基丁酸的含量的分析方法。采用乙腈萃取血液样品,经BEH C18色谱柱(2.1×50 mm,1.7μm)分离,以0.1%甲酸水溶液(含0.5%乙酸胺):乙腈(95:5,V/V)为流动相,流速0.2 m L/min,质谱检测器(QDa)检测,正离子SIR模式,m/z=104进行定量,进样量1μL。对照品在0.5~10μg/m L浓度范围内与峰面积线性关系良好。3个添加试验的平均回收率分别为78.9%,87.6%,79.5%,RSD分别为1.2%,1.1%,2.1%。     

枞酸乙二醇单酯与双酯的合成工艺研究

采用L39^4正交实验研究了枞酸乙二醇单酯与双酯的合成工艺。探讨了反应温度、催化剂用量、反应物料摩尔比、反应时间等诸因素对转化率及选择性的影响。结果表明：反应温度与反应物料摩尔比分别对转化率及选择性具有最显著的影响。实验提供了枞酸乙二醇单酯与双酯的优化合成条件,在此基础上以松香为原料进行了验证。     

聚对苯二甲酸乙二醇酯/聚乙二醇醚插层嵌段共聚物的结晶性能

合成了不同用量、不同分子量的聚乙二醇醚(PEG)或聚丁二醇醚(PTMC)与聚对苯二甲酸乙二醇酯(PET)/蒙脱土(MMT)的嵌段共聚物。研究了MMT在共聚物中的分散状态及PEG或PTMG对PET/MMT插层聚合物结晶性能的影响。结果表明,MMT在共聚物中以纳米尺寸分散;加入PEG或PTMG增强了聚酯链段的柔顺性,使共聚物熔体降温过程的结晶温度提高,冷结晶温度降低,即插层嵌段共聚物的结晶速率提高;在合成的共聚物中,分子量为2000,用量为DMT的6%的PEG对插层共聚物结晶速率的促进作用最大     

油酸乙二醇酯添加剂中双酯组成的气相色谱-质谱分析

用硅胶玻璃色谱柱吸附样品 ,采用溶剂梯度洗脱的方法从油酸乙二醇酯添加剂中分离出乙二醇双酯 ,再用GC -MS详细地分析了乙二醇双酯的组分 ,给出了分析乙二醇双酯的优化条件 ,并通过乙二醇双酯的组分推断出油酸原料中所含酸的种类。     

气相色谱-质谱联用法同时测定烟草中的1-丙醇、二甘醇、三甘醇、丙二醇与丙三醇

将烟草样品粉碎至40目,以1,4-丁二醇为内标,甲醇为萃取溶剂,超声萃取60 min后,以气相色谱-质谱/选择离子监测(GC-MS/SIM)法测定1-丙醇、二甘醇、三甘醇、丙二醇和丙三醇的含量。结果表明:目标化合物在1~100μg/mL范围内线性关系良好,方法的检出限为0.05~0.48μg/mL,回收率为90.2%~103.7%,相对标准偏差(RSDs)为0.9%~3.0%。方法的前处理简单、灵敏度高、定性定量准确,适用于烟草中多元醇的定性定量分析。     

Thiocyanatoarylation of Diethylene Glycol Diacrylate

The example of diethylene glycol diacrylate was used to demonstrate the possibility of thiocyanatoarylation both by one and by two multiple bonds of compounds with two isolated multiple bonds. The reactions of arenediazonium tetrafluoroborates with diethylene glycol diacrylate in aqueous acetone (1:2) in the presence of catalytic amounts of copper gave 1-acryloyloxy-2-[2-(2-thiocyanato-3-arylpropionyloxy)ethoxy]ethanes. The latter were reacted with arenediazonium tetrafluoroborates in aqueous acetone (1:3) to obtain 1-[2-(2-thiocyanato-3-arylpropionyloxy)ethoxy]-2-(2-thiocyanato-3-arylpropionyloxy)ethanes via thiocyanatoarylation by two multiple bonds.     

熔化提取-毛细管气相色谱法测定乙二醇硬脂酸酯中乙二醇的残留量

提出了毛细管气相色谱法测定乙二醇硬脂酸酯中乙二醇残留量的方法。样品在50℃熔化,经甲醇超声浸提,以丙二醇为内标,采用HP-5毛细管色谱柱分离,用火焰离子化检测器测定。乙二醇的质量浓度在102.6~1 026.0 mg.L-1范围内呈线性,方法的检出限(3S/N)为30 mg.L-1。应用此方法分析乙二醇硬脂酸酯,回收率在93.7%~103.2%之间。     

Determination of Polyethylene Glycol Monoester Acrylate and Polyethylene Glycol Diester Acrylate Using Reversed-Phase High-Performance Liquid Chromatography

A procedure was developed for the determination of polyethylene glycol monoester acrylate (PEGMA) and polyethylene glycol diester acrylate (PEGDA) by reversed-phase high performance liquid chromatographic (RP-HPLC) with UV detector. Sample was well separated on an SinoChrom ODS-BP (C-18) column (200 × 4.6 mm i.d., 5 μm) with mobile phases composed of acetonitrile-phosphate buffer solution (0.05 mol · L^?1 pH = 6.86) in the ratio of 42:58 (v/v). The PEGMA and PEGDA were detected by UV detector at 205 nm, and quantitatively analyzed with an external standard of methyl acrylate. For PEGMA, the linear response ranged from 0.40 × 10^?5 mol · L^?1 to 2.00 × 10^?3mol · L^?1 (r² > 0.999), the detection limit was 0.12 × 10^?5 mol · L^?1, the recovery rate was found to be 93.4%–99.7%. For PEGDA, the linear response ranged from 0.20 × 10^?5 mol · L^?1 to 1.00 × 10^?3mol · L^?1 (r² > 0.999), the detection limit was 0.04 × 10^?5 mol · L^?1, the recovery rate was found to be 99.1% ～ 105.8%. This quantitative method can also be used in the HPLC analysis of other α,β-unsaturated esters.     

Novel Biotreatment Process for Glycol Waters

Propylene oxide (PO), propylene glycol (PG), and polyols are produced from propylene via propylene chlorohydrin. Effluents from these plants contain biological oxygen demand/chemical oxygen demand (BOD/COD) loads besides high chloride concentrations. The high salinity poses severe problem to adopt conventional methods like activated sludge processes. Presently, a simple, economically viable and versatile microbiological process has been developed to get more than 90% biodegradation in terms of BOD/COD, utilizing specially developedPseudomonas andAerobacter. The process can tolerate high salinity up to 10 wt% NaCl or 5 wt% CaCl₂ and can withstand wide variations in_pH (5.5–11.0) and temperature (15–45°C). The biodegradation of glycols involves two steps. The enzymatic conversion of glycols to carboxylic and hydroxycarboxylic acids is aided byPseudo- omonas. Further degradation to CO₂ and H₂O by carboxylic acid utilizingAerobacter, and possible metabolic degradative pathway of glycols are discussed. Various process parameters obtained in the lab scale (50 L bioreactor) and pilot scale (20 m³ bioreactor), and unique features of our process are also discussed.     

Microwave—activated Coupling Reaction on Polyethylene Glycol

The two-step Sonogashira coupling reaction took place rapidly under microwave activation condition. PEG bound substrates acted as PTC and polymer support as well. Its yields are 80-90% and the products are in high purity.