Determination of Pentachlorophenol Laurate by High Pressure Liquid Chromatography

Abstract

Pentachlorophenol Laurate (PCPL) in canvas is determined by extraction and chromotography on silica gel. Conditions are chosen to eliminate peak splitting due to the presence of different “laurate” fatty acids. The determination is faster and more specific than previously reported methods.     

Determination of Amikacin Isomers by High Pressure Liquid Chromatography

Abstract

A high-pressure liquid chromatographic (HPLC) method for quantitative monitoring of amikacin isomers is described. Four isomers, BB-K8, BB-K29, BB-K6 and BB-K11 were applied to a silica gel column. While adsorbed, the isomers were derivatized with o-phthalaldehyde and the derivatized products eluted with ethanol. A decrease in the fluorescence of the derivatized products with time was observed. Heating at 50°C for 5 min produced products with stable fluorescence for at least three hours. Using the fluorescent properties of the amikacin derivative for detection, the four isomers of amikacin were separated by reverse phase (HPLC). A linear relationship from 1 to 10 μg/mL was obtained for all four isomers.     

痕量神经肽的高效液相色谱

本文选用芴甲氧羰基氯(FMOC-CL)作为肽的荧光衍生试剂,建立了两段淋洗分离测定神经肽RP-HPLC的方法。衍生反应简便、快速、衍生物稳定。FMOC-脑啡肽、FMOC-P物质在18min内全部被洗脱。本方法在1～100pmol具有良好的定量线性关系。当信噪比为2.5:1时,检测极限:FMOC-甲硫脑啡肽为405fmol,FMOC-亮脑啡肽337fmol,FMOC-P物质为500fmol。并且能够容易地脱去衍生基团得到反应前的神经肽。     

Simultaneous Determination of Salicylic Acid and Salicyluric Acid in Plasma and Urine by High Pressure Liquid Chromatography

Abstract

A sensitive, rapid, and specific high pressure liquid chromatographic (HPLC) assay was developed for the determination of salicylic (SA) and salicyluric (SU) acids in plasma and urine. The compounds are extracted into ethyl ether at acid pH, evaporated, and reconstituted prior to instrumental separation. Overall recovery of both compounds is 90 ± 5%, and the sensitivity limits are 150 ng of SU and 300 ng SA per ml of biological fluid. The assay was used for the determination of both compounds in plasma and urine of man following oral doses of 40 mg/kg of sodium salicylate.     

高效液相色谱法同时测定虫草素和腺苷

本文用微波法提取蛹虫草培养基和子实体中的虫草素及腺苷,并利用高效液相色谱法同时测定虫草素和腺苷.选择Inertsil ODS-SP柱(150×4.6 mm,5 μm)为色谱柱,乙腈-水为流动相,流速1.0 mL/min,柱温35℃,二极管阵列检测器(DAD)检测,检测波长260 nm,进样量10 μL.在2～10 μg...     

Determination of Sterigmatocystin in Fungal Cultures by High Pressure Liquid Chromatography

Abstract

Levels of sterigmatocystin in cultures of various fungal strains were determined by high pressure liquid chromatography (HPLC). This mycotoxin was well separated using acetonitrile / water / acetic acid (55/45/2) as solvent on a μ-Bondapak C18 column (Waters Associates). It was detected by its absorbance at 320 nm. Using this method, sterigmatocystin can thus be simply and rapidly determined in mould strain cultures.     

Urinary Uric Acid Determination by Reversed-Phase High Pressure Liquid Chromatography

Abstract

Reversed-phase high pressure liquid chromatography with UV detection was proven to be a powerful method for the separation and quantitation of urinary uric acid. We have compared three different treatments for urine samples previous chromatographic injection: alkaline methanol extraction, ethylacetate extraction and centrifugation. It was also studied storage conditions for urine samples.

Our findings show that the method has high specificity and reproducibility for urinary uric acid. Samples are stables and require only centrifugation previous injection to the chromatograph.     

高效液相色谱法同时测定多种食品添加剂

 采用反相高效液相色谱法 ,一次进样、同时测定食品中的人工合成甜味剂 (糖精钠、安赛蜜、甜味素 )、防腐剂(苯甲酸、山梨酸 )、咖啡因、可可碱和茶碱。以AlltechEconosphereC18柱 (15 0mm× 4 6mmi.d .,3μm)为分离柱 ,10mmol/LNaH2 PO4 (pH 4 0 0 ) 乙腈 (体积比为 90∶10 )为流动相 ,采用二极管阵列检测器进行检测。整个分离过程在 2 3min内完成。样品平均加标回收率为 78 5 %～ 10 7 2 %。     

5种甜味添加剂的反相高效液相色谱法同时测定

建立了同时测定5种人工合成甜味剂阿斯巴甜、糖精钠、甜蜜素、安赛蜜、纽甜的反相高效液相色谱分析方法.以Synergi Fusion-RP柱为分离柱,20mmol/L硫酸铵缓冲溶液(pH 4.4)-乙腈为流动相,梯度洗脱.采用二极管阵列检测器进行检测,整个分离过程在9min内完成.样品加标回收率为89%～107%;相对标准偏差小于3.2%.该法可用于食品和饮料中5种甜味剂的同时测定.     

Simultaneous Determination of Six Anticonvulsants in Serum by High Performance Liquid Chromatography

Abstract

The authors describe a simultaneous determination method of six anticonvulsants (ethosuximide, primidone, phenobarbital, phenytoin, carbamazepine, valproic acid) using 500 μl of serum.

After the addition of the internal standard (5-(p-methylphenyl)-5 phenylhydantoin), the anticonvulsants are extracted in an acid medium with ethyl acetate. They are separated by reverse phase chromatography on a μ Bondapack C18 column, eluted with a water/methanol mixture (36/64 V/V) at a flow rate of 0.7 ml/min.

The column effluent is first analyzed by monitoring the ultraviolet absorption at 197 nm and then at 425 nm after the addition of a color indicator: bromocresol purple. The analysis lasts 12 minutes at ambient temperature. The sensitivity obtained with the serum for the range of products investigated is of the order of 0.5 to 2 mg/l, the extraction recoveries varying from 75 to 100% depending on the drug. Reproducibility is good (cv ≤ 9%).     

高效液相色谱法对唇膏中9种限用着色剂的同时测定

建立了用高效液相色谱/二极管阵列检测器(HPLC/DAD)同时测定唇膏中9种限用着色剂(溶剂绿7、食品黄3、食品红17、酸性黄1、酸性红33、食品红4、食品红1、橙黄Ⅰ和酸性橙7)的检测方法.采用C18反相色谱柱,以乙腈-磷酸二氢钾缓冲溶液(pH 6.0)为流动相进行梯度洗脱,用DAD检测器扫描检测.以保留时间结合待测物的紫外吸收光谱进行定性分析,采用外标法进行定量分析,定量检测波长240 nm.所建方法可在15 min内对9种目标物同时进行检测,且各化合物均达到基线分离.实验结果表明,在0.05 ～100 mg/L范围内,9种着色剂的质量浓度与相应的峰面积比值呈良好的线性关系.方法的平均回收率(n=9)为85% ～100%,相对标准偏差(RSD)为3.68% ～8.20%,9种目标物的检出限为0.01 ～0.1 mg/L.     

饲料中四环素类药物含量的高效液相色谱测定

建立了高效液相色谱法测定饲料中四环素类药物含量的方法。样品经甲醇-盐酸溶液提取,WatersOasis HLB固相萃取柱净化,进行HPLC分析。标准校正曲线线性范围为0.05~2.0 mg/L,相关系数r>0.999。饲料中土霉素、四环素、金霉素和强力霉素的定量下限(LOQ)依次是2.0、2.0、4.0和4.0 mg/kg;不同添加水平样品加标回收率为78%~103%,RSD小于11%。     

高效液相色谱法对化妆品中17种致敏原的同时测定

建立了同时测定化妆品中17种致敏原(茴香醇、苯甲醇、香豆素、肉桂醇、丁香酚、异丁香酚、香叶醇、芳樟醇、柠檬醛、2-辛炔酸甲酯、戊基肉桂醇、水杨酸苄酯、肉桂酸苯甲酯、戊基肉桂醛、α-异甲基紫罗兰酮、α-己基肉桂醛、苧烯)的高效液相色谱方法。不同类型的化妆品样品经无水乙醇超声提取,以15000 r/m in离心15 min,取上清液过滤后测定。采用Agilent ZORBAX Ec lipse XDB-C8(4.6 mm×250 mm,5μm)色谱柱,以乙腈-水为流动相梯度洗脱,流速1.0 mL/min,采用二极管阵列检测器多波长检测(210、230、250、275、300 nm)。17种致敏原的定量下限为10~500μg/kg,线性范围内相关系数均大于0.999。在高、中、低3个添加水平下的平均加标回收率(n=5)为85%~118%,相对标准偏差为1.5%~9.7%。该方法简便、快速、准确,适用于化妆品中17种致敏原的测定。     

高效液相色谱法同时测定纺织品中四氯苯酚同分异构体及五氯苯酚和邻苯基苯酚

建立了高效液相色谱法同时测定纺织品中四氯苯酚同分异构体(2,3,4,5-TeCP、2,3,4,6-TeCP、2,3,5,6-TeCP)及五氯苯酚(PCP)和邻苯基苯酚(OPP)的分析方法。样品经甲醇超声提取、浓缩后,采用Symmetry C18色谱柱,以甲醇-10mmol/L乙酸铵溶液为流动相,梯度洗脱,二极管阵列检测器210nm检测。结果表明:三种TeCP同分异构体及PCP、OPP在0.1~20mg/L范围内具有良好的线性关系,相关系数为0.9994~0.9998,样品加标回收率为87.2%~109%,相对标准偏差为0.92%~4.50%,方法的最低检测浓度分别为0.05、0.10、0.05、0.05、0.05mg/kg。该方法高效、简便、准确可靠,可实现现行法规所要求的纺织品中苯酚类物质的同时测定。     

高效液相色谱同时测定鸡蛋中4种氟喹诺酮类药物残留

建立了固相萃取—反相高效液相色谱同时分析鸡蛋样品中4种氟喹诺酮类药物残留量的方法。对鸡蛋样品的提取及其在C18固相萃取柱上的净化条件进行了研究,采用高效液相色谱分离,荧光检测器检测(λex=280nm,λem=450nm),外标法定量。4种沙星标准曲线的线性回归系数均在0．9999以上,环丙沙星、恩诺沙星、沙拉沙星的线性范围为2．5～500μg／L;达诺沙星为0．5～100μg/L。鸡蛋样品中4种沙星的加标回收率为78．1％～95．7％;相对标准偏差为4．1％～16．2％。环丙沙星、恩诺沙星、沙拉沙星的最低检出限为10μg／kg;达诺沙星的最低检出限为2μg/kg。     

高效液相色谱法对化妆品中17种香豆素类化学成分的同时测定

建立了同时测定化妆品中17种香豆素类化学成分(双香豆素、7-羟基-6-甲氧基香豆素、8-羟基补骨脂素、香豆素、6,7-二甲氧基香豆素、二氢香豆素、7-甲氧基香豆素、7-甲基香豆素、补骨脂素、8-甲氧基补骨脂素、5-甲氧基补骨脂素、4-甲基-7-乙氧基香豆素、2′,4,8-三甲基补骨脂素、欧前胡素、异欧前胡素、二氢欧山芹醇当归酸酯、环香豆素)的高效液相色谱分析方法。样品经甲醇超声提取,以8 000 r/min离心15 min,取上清液过滤后测定。采用Agilent Zorbax SB-Phenyl柱(4.6 mm×250 mm,5μm)分离,以水-甲醇-乙腈三元流动相梯度洗脱,流速1.0 mL/min,柱温30℃。采用二极管阵列检测器多波长检测(210、220、250 nm),外标法定量。17种香豆素类化合物的定量下限(LOQ)为1 mg/kg,线性范围为0.5~60 mg/L,相关系数(r)均大于0.999。在高、中、低3种加标水平下的平均加标回收率(n=6)为86%~106%,相对标准偏差为0.3%~3.6%。该方法准确、简便,适用于化妆品中17种香豆素类化合物的测定。     

高效液相色谱法同时测定纺织品中10种酚类化合物

建立了高效液相色谱法同时测定纺织品中五氯苯酚、2,3,4,5-四氯苯酚、2,3,4,6-四氯苯酚、2,3,5,6-四氯苯酚、2,4,5-三氯苯酚、2,4,6-三氯苯酚、邻苯基苯酚、间羟基联苯、2-萘酚、对硝基苯酚10种酚类化合物的检测方法。纺织品中的酚类化合物经甲醇超声提取、浓缩后,以ZORBAX SB-C18柱(4.6 mm×150 mm,5μm)为分析柱,乙腈和0.01 mol/L磷酸溶液为流动相梯度洗脱,采用二极管阵列检测器,在220 nm和310 nm波长下进行高效液相色谱检测,紫外光谱库确证,外标法定量。10种酚类化合物在0.3～37 mg/L浓度范围内与其峰面积呈良好的线性关系,相关系数为0.999 1～0.999 5;以不低于3倍的信噪比计算10种酚类化合物的检出限(LOD)为0.003 0～0.041 1 mg/kg;定量下限(LOQ,S/N≥10)为0.010 0～0.1370 mg/kg。棉、麻、毛3种纺织品基质在3个不同加标水平的回收率为81%～105%,相对标准偏差(RSDs)为1.7%～8.5%。该方法能同时完成10种酚类化合物的确证和分析,可用于纺织品中酚类化合物残留的检测分析。     

高效液相色谱法同时检测化妆品中两种亚硝基物质

建立了同时测定化妆品中4-亚硝基苯酚和1-甲基-3-硝基-1-亚硝基胍两种亚硝基类禁用物质的高效液相色谱方法。化妆品样品经溶剂超声提取,经Fortis-C18柱分离,二极管阵列检测器(DAD)检测,保留时间定性,外标法定量。实验结果表明:该方法在0.5～10μg/mL浓度范围内,两种物质均具有良好的线性响应,方法对4-亚硝基苯酚和1-甲基-3-硝基-1-亚硝基胍的检出限均为20ng/g,在三个添加水平下的平均回收率分别在94.14%～102.8%和96.3%～104.1%之间,相对标准偏差(RSD)均<3.5%。     

高效液相色谱法同时测定血清中的犬尿氨酸和色氨酸

建立了一种能同时检测血清中的犬尿氨酸(kynurenine,Kyn)和色氨酸(tryptophan,Trp)的高效液相色谱-紫外检测法。采用的色谱柱为Symmetry Shield RP-C18柱(150 mm×3.9 mm i.d.,5 μm),流动相为15 mmol/L乙酸钠-乙酸溶液(含2.7%乙腈,pH 3.6),流速为1.0 mL/min,紫外检测波长为225 nm。血清标本经5.0%(体积分数)高氯酸溶液去除蛋白质后取上清液直接进样分析测定。研究结果表明,Kyn保留时间为3.5 min,线性范围为0.098~49 μmol/L,最低检出浓度为0.02 μmol/L,回收率为90.82%~93.45%;Trp保留时间为8.1 min,线性范围为4.9~490 μmol/L,最低检出浓度为0.20 μmol/L,回收率为95.51%~98.67%。Kyn和Trp日内、日间测定的相对标准偏差均小于4%,苯丙氨酸、酪氨酸、5-羟色胺和犬尿喹啉酸等物质对该法均无干扰。该方法简便、快速、稳定、可行,可应用于临床和科研工作。     

高效液相色谱法同时测定香兰素与邻位香兰素

建立了同时测定香兰素和邻位香兰素的高效液相色谱法.考察了流动相组成、柱温等因素对分析效率的影响.在流动相为5% 乙酸-乙腈(60 :40,体积比),流速1.0 mL/min,柱温25 ℃的优化条件下,香兰素和邻位香兰素可在5 min内实现分离.测定结果表明,香兰素和邻位香兰素在10 ～240 mg/L范围内线性关系良好...