Determination of propyl gallate in edible oil by high-performance liquid chromatography with chemiluminescence detection

A novel and convenient method based on high-performance liquid chromatography coupled with chemiluminescence (HPLC) for the determination of propyl gallate in edible oil is reported. The detection was based on the inhibition of chemiluminescence between luminol and hydrogen peroxide in alkaline solution. The analysis was performed using a C₁₈ column with isocratic 60:40 methanol/water. Under the optimum conditions, the concentration of propyl gallate was linear from 9?×?10^?6?mol?L^?1 to 1?×?10^?4?mol?L^?1 with a detection limit of 2?×?10^?7?mol?L^?1. The method is simple, sensitive, and inexpensive and was used for the determination of propyl gallate in edible oil.     

Determination of baicalin in cosmetics and toothpaste by solid-phase extraction and high-performance liquid chromatography

Baicalin was determined in cosmetics and toothpaste by high-performance liquid chromatography. The samples were extracted with ultrasound in 75% ethanol for 20 min, purified by anion exchange solid-phase extraction cartridge, and the components were separated on a C18 column. The limits of detection and quantification were 3.0 mg kg^?1 and 10.0 mg kg^?1. The recovery was from 81.3–101.6%. A linear relationship was present from 1.00–100 µg · mL^?1 of baicalin. The protocol was simple, sensitive, selective, and used to determine baicalin in personal care products. Baicalin was not present in materials contrary to the labeled contents.     

Determination of benzimidazoles in pharmaceuticals and human serum by high-performance liquid chromatography

A liquid chromatographic method is described for the quantification of prednisolone, benzimidazoles, and preservatives using a C₁₈ analytical column as stationary phase. The mobile phase was 30:70 methanol:pH 2.5 phosphate buffer at a flow rate of 1.0 mL min^?1 with absorbance detection at 235 nm. The method was linear for concentrations ranged from 40–10,000 ng mL^?1. Low values of coefficient of variance were obtained when samples were analyzed as replicates. Excellent recovery values were recorded in commercial products and fortified samples. International Conference of Harmonization protocols were employed to perform comprehensive method validation. The reported method has applications for pharmaceutical and serum samples.     

Determination of phenolic acids and rutin in Heliotropium thermophilum by high-performance liquid chromatography with photodiode array detection

A novel and rapid method was validated for the determination of phenolics in plants by high-performance liquid chromatography coupled to photodiode array detection. The optimized method was employed for the quantification of phenolic acids and rutin present in Heliotropium thermophilum. Eight samples collected from two locations were analyzed. Additionally, temperature dependent changes in the phenolic composition of H. thermophilum samples was evaluated. A series of standards were used for identification that included gallic acid, protocatechuic acid, 4-hydroxybenzoic acid, chlorogenic acid, vanillic acid, caffeic acid, syringic acid, p-coumaric acid, rutin, ferulic acid, benzoic acid, 2-hydroxycinnamic acid, abscisic acid, and trans-cinnamic acid. Chromatographic separation was performed on C₈ column at 40°C with gradient elution. A phosphate buffer (20 mM, pH: 2.5) and acetonitrile mixture was used as the mobile phase with detection at 280 nm wavelength and a flow rate of 1.5 mL/min. The developed method was shown to be sensitive, accurate, and reproducible for the determination of phenolic acids and rutin in plants.     

反相高效液相色谱法测定打印机喷墨中的苯酚

本文采用氯仿萃取 ,反相键合相C8柱测定打印机喷墨中的苯酚 ,线性范围 :0 4～ 2 0 0 μg/mL ,r =0 9995 ,精密度 0 39% ,天内误差 :0 97% ,天间误差 :1 72 %。该法可在 6min内完成测定。     

Determination of triacylglycerols in food by high-performance liquid chromatography

Food contamination is a major global issue and the challenges are increasing. Alternative methodology using lipids in detecting contaminants and determining food ingredients is needed to supplement or replace current methodology. The core–shell column is considered to be a breakthrough for high-performance liquid chromatography. In this study, lipid profiling was performed using a C18 core–shell column to separate and identify triacylglycerols in oil and food. The chromatographic profiles were compared at various flow rates to determine their efficiency. The evaluation was done based on chromatographic resolution, resolving power, and separation efficiency. In addition, the height equivalent to a theoretical plate of the column was determined and a comparison was made at the same linear velocity along with the peak capacity. The most efficient flow rate was 400?µL/min, and by applying the methodology, triacylglycerols from edible oil and food were extensively profiled. The results show that triacylglycerol profiles may be utilized as a biomarker for food quality. This alternative methodology provided a comprehensive profile of triacylglycerols in oil and food that allowed the identification of unique triacylglycerol biomarkers for practical analysis.     

Determination of protoberberine alkaloids in Coptidis Rhizoma by novel extraction and high-performance liquid chromatography

An alternative, effective, and solvent-free microextraction method has been developed using weighing paper as the adsorbent for five protoberberine alkaloids from the methanolic extract of Coptidis Rhizoma (C. Rhizoma). Several variables influencing extraction efficiency were optimized. 1.0?×?1.0?cm glassine weighing paper was employed for the isolation of the analytes followed by high-performance liquid chromatography. Under the optimum conditions, the limits of detection were between 0.2 and 0.4?ng/mL with enrichment factors from 41–47. The calibration curves were linear across the concentration ranges examined with correlation coefficients exceeding 0.992. All relative standard deviations were less than 10.0%. The method was employed for the determination of the analytes in C. Rhizoma. Berberine, palmatine, coptisine, epiberberine, and jatrorrhizine were present at concentrations between 9.62?±?0.87?mg/g and 0.48?±?0.05?mg/g.     

高效液相色谱法检测小麦粉中的偶氮甲酰胺方法的研究

小麦粉中偶氮甲酰胺(azodicardonamide,ADA)用丙酮提取,提取液氮吹浓缩后用5%二甲基亚矾的水溶液定容,并用正己烷脱脂。样品供高效液相色谱仪测定,外标法定量。方法线性范围是0～100mg/L(r~2=0.9979),定量下限为4mg/kg。在小麦粉基质粉中分别添加10.0mg/kg、50.0mg/kg两个水平的偶氮甲酰胺标准品,方法的回收率为84%～90%,相对标准偏差小于5%。     

高效液相色谱法测定大鼠全血中的灵芝酸单体Me

建立大鼠全血中灵芝酸单体Me的高效液相色谱测定方法。采用色谱柱Diamonsil~(?)C_(18)柱(250mm×4.6μm,5μm),流动相为甲醇-水(体积比为94:6,用醋酸调pH至3.6);流速为1mL/min;检测波长为245nm;内标为苯丙酸诺龙。灵芝酸单体Me血中浓度在0.05～40μg/mL范围内线性良好(r>0.99),定量限为50ng/mL,日内和日间测定的精密度(以相对标准偏差表示)均低于8.6%。该方法简便、灵敏、准确,适用于大鼠体内灵芝酸的药物动力学研究。     

高效液相色谱法测定甘蓝、青菜和番茄中虫酰肼、甲氧虫酰肼和呋喃虫酰肼残留

建立了同时测定蔬菜（甘蓝、青菜和番茄）中虫酰肼、甲氧虫酰肼和呋喃虫酰肼（福先）农药残留的高效液相色谱法。以酸化甲醇高速匀浆提取，正己烷去除脂类杂质，二氮甲烷反革取去除亲水性杂质，再经氟罗里硅土柱层析净化，效果显著。采用甲醇-水（75＋25，V／V）为流动相，利用Agilent HC—C18柱和紫外检测器（检测波长：230nm）对待测组份进行了分离和测定。实验证明，添加浓度在0．05mg／kg，0．2mg／kg和1mg／kg时，蔬菜（甘蓝、青菜和番茄）中虫酰肼、甲氧虫酰肼和呋喃虫酰肼平均添加回收率在76．9％～105％之间，相对标准偏差（RSD，n=5）小于10％，虫酰肼、甲氧虫酰肼和呋喃虫酰肼在样品中的最低检出浓度为0．05mg／kg。     

正相高效液相色谱法检测火箭煤油中的芳烃

在ASTM6379标准方法的基础上,建立火箭煤油中芳烃的液相色谱-紫外检测方法。该方法采用氨基柱串联氰基柱,以正己烷为流动相,流速1.0mL/min,柱温28℃。单环芳烃以邻二甲苯计在8~80mg/L（r2=0.9999）范围内线形关系良好,定量限0.008mg/L,在已知浓度的样品溶液中分别加入高、中、低3种不同浓度的标准品溶液,回收率85.4%~114.1%,相对标准偏差小于5%。该方法简便易行、准确可靠。     

离子色谱-紫外检测法测定牛奶中的三聚氰胺

建立离子色谱-紫外法检测牛奶中三聚氰胺的方法。利用乙腈沉淀牛奶中的蛋白,十八烷基(ODS)固相萃取柱对上清液中的三聚氰胺进行富集。选用SH-Cation 2阳离子交换色谱柱,以甲烷磺酸(MSA)作淋洗液,240nm紫外波长下进行检测。该法在0.10～10.0mg/L范围内线性关系良好,R~2为0.9998,检测限为0.50 μ g/L,加标回收率在92.0%～99.8%之间。方法简便易行,灵敏度高,结果准确。     

液相色谱串联质谱法测定动物组织中大环内酯类残留量

采用高效液相色谱-电喷雾串联质谱仪（LC -ESI-MS-MS）,建立猪肉中林可霉素、竹桃霉素、替米考星、泰乐菌素、克林霉素、吉他霉素、交沙霉素等7种大环内酯类药物残留的检测方法,试验中猪肉中大环内酯类抗生素的残留用乙腈提取,以罗红霉素作为内标,提取液用正己烷去除脂肪后浓缩,再用磷酸盐溶液溶解后,经HLB固相萃取柱净化,甲醇洗脱,洗脱液浓缩定容至1mL ,供液相色谱-串联质谱法测定,内标法定量。本方法采用10μg/kg ,20μg/kg ,100μg/kg ,3个添加浓度,每个浓度6个平行样品,上述7种大环内酯类药物残留的回收率在75％～100％,相对偏差在1.51％～5.48％。     

固相萃取-高效液相色谱法测定水中甲萘威

采用固相萃取，高效液相色谱法对水中甲萘威进行检测，通过实验研究，该法对水中甲萘威的最低检测限为0．001mg/L，相对标准偏差（RSD，n=5）≤2．5％，加标回收率为98．0％～98．5％，固相萃取效果优于液液萃取。该方法适合于地表水及饮用水中甲萘威的检测。     

HPLC-ICP-MS联用技术测定玩具中痕量可迁移有机锡

建立了高效液相色谱-电感耦合等离子体质谱 (HPLC-ICP-MS) 联用技术测定玩具中痕量可迁移有机锡的方法。采用Waters Acquity UPLC HSS T3分析柱,在流动相为V（乙腈）∶V(水)∶V (乙酸)=65∶23∶12的混合溶液中加入0.1%三乙胺作为离子对试剂,在pH 3.0条件下,可以很好地分离二丁基锡（DBT）、三苯基锡（TPhT）、三丁基锡（TBT）和二辛基锡（DOT）。此方法简便、快速、灵敏度高,在50 μL进样量下,DBT、TPhT、TBT及DOT的检出限分别为0.08、0.24、0.14和0.65 μg/L;在5、50 μg/L两个加标水平下,回收率分别为80.7%~96.3%和83.5%~100.4%,方法精密度优于4.7%,可以满足测定要求。应用该方法测定了玩具可接触部分材料,包括织物、木料、塑料、涂层中的可迁移有机锡,分析结果令人满意。     

加速溶剂萃取法结合HPLC-ESI-TOF MS测定清肝散结汤中29种化学成分

清肝散结汤（QGSJ）是由14味不同中药组成的复方制剂,基于长期的实验观察和临床经验以不同组合成方用于肝癌的治疗。本研究建立了一种基于加速溶剂萃取（ASE）结合高效液相色谱-电喷雾飞行时间质谱（HPLC-ESI-TOF MS）的方法同时测定清肝散结汤中29种化学成分。使用70%乙醇作为提取溶剂,提取温度100 ℃,静态萃取时间5 min,提取2次,以上条件采用正交设计和主成分分析进行优化。HPLC分离采用Kromasil C18色谱柱,梯度洗脱。TOF MS在负离子模式下检测,质量扫描范围m/z 100~1100。结果表明：清肝散结汤中29种成分具有良好的线性关系（r＞0.994）和日内、日间精密度（RSD＜5%）;提取回收率在96.5%~104.5%之间。该方法快速、可靠,适用于复方中药的定量评价。     

凝胶色谱净化-毛细管气相色谱法测定渔业水体中乐果

建立凝胶色谱净化-毛细管气相色谱法测定养殖水体中乐果的分析方法。三氯甲烷萃取水样,经凝胶渗透色谱(GPC)净化除去脂类、色素等,采用脉冲不分流进样模式气相色谱法分析,外标法定量。方法检测限为0.022μg/L;加标水平为1.00μg/L时,实际样品回收率为82.5%～97.1%。该方法自动化程度高、净化效果好、重现性好、准确灵敏。实际样品检测结果表明,此方法满足复杂水体中乐果残留检测要求。     

反相高效液相色谱法测定水果中有机酸含量

利用反相高效液相色谱法同时测定苹果、梨、橙子中草酸、酒石酸、乙酸、乳酸4种有机酸的含量.采用Waters2695 HPLC-PDA色谱系统,Waters Xbridge C18(4.6×250mm,5 μm)色谱柱,乙腈和0.01 mol/L磷酸二氢钠溶液(pH=2.6)作为流动相,流速1.00mL/min,柱温30℃,紫外检测波长214nm的色谱条件下,能够在10分钟内较好地定量分析水果中4种有机酸的含量,本方法回收率为92.17％-103.19％,相对标准偏差为0.23-0.65,各有机酸标准曲线相关系数均在0.9997以上.本方法准确、高效,灵敏度高,适用于水果中有机酸的检测.     

液相色谱-同位素稀释质谱法测定血清生长激素

复杂基质中低丰度蛋白质的准确定量分析一直是蛋白质研究的重点和难点.随着质谱技术的飞速发展,同位素稀释质谱法成为血清中低丰度蛋白质准确定量分析的重要方法.本研究以同位素标记的人生长激素为内标,通过C12和C4色谱柱两次分离收集目标馏分,建立了基于离线二维高效液相色谱分离血清样本的新方法.然后,结合高效液相色谱-同位素稀释...     

固相萃取-高效液相色谱法测定水中12种酚类化合物

采用固相萃取,高效液相色谱分离,紫外分光光度法对水中12种酚类物质进行检测。通过实验研究,该法对12种酚的最低检测限为0.17~0.56μg/L,相对标准偏差(RSD,n=7)小于等于6.5%,加标回收率为86.67%~106.33%。该方法适合于地表水及饮用水中酚类化合物的检测。