Simultaneous high-performance liquid chromatographic determination of paracetamol, phenylephrine HCl, and chlorpheniramine maleate in pharmaceutical dosage forms

A rapid, precise, and specific high-performance liquid chromatographic method is described for the simultaneous determination of paracetamol, phenylephrine HCI, and chlorpheniramine maleate in combined pharmaceutical dosage forms. The method involves the use of a microBondapak CN RP analytical column (125 A, 10 microm, 3.9 x 150 mm) at 22 degrees C as the stationary phase with the mixture of acetonitrile and phosphate buffer (pH 6.22, 78:22) as the mobile phase. Derivatization of the drugs is not required. The method is applied to commercial pediatric cough-cold syrups, tablets, and capsules marketed in Turkey. The relative standard deviation for 10 replicate measurements of each drug in the medicaments is always less than 2%.     

气相色谱法直接测定植物生长素

 建立了一种采用 5 3 0 μm大口径毛细管色谱柱、不经衍生化处理而直接测定吲哚乙酸 (IAA)、吲哚丁酸(IBA)和萘乙酸 (NAA)等植物生长素的气相色谱分析方法。以邻苯二甲酸二丁酯为内标物 ,用 FID检测 ,IAA,IBA和 NAA的相对标准偏差分别为 1 .1 4% ,0 .61 %和 0 .78%。方法简便、快速、准确、重现性好 ,可用于生长素类单组分和混合制剂的质量检测。     

高效液相色谱同时测定3类食品中的5种罂粟壳生物碱

建立了同时检测3类食品中吗啡、可待因、蒂巴因、罂粟碱、那可汀5种罂粟壳生物碱含量的高效液相色谱法.试样经无水乙醇超声提取,Waters-C18(4.6 mm ×250 mm,0.5 μm)柱分离,以甲醇-0.01 mol·L-1磷酸盐为流动相梯度洗脱,通过紫外检测器进行检测.5种罂粟壳生物碱的质量浓度在10～600 m...     

Simultaneous determination of some active ingredients in cough and cold preparations by gas chromatography, and method validation

A simple and rapid gas chromatographic (GC) method has been developed for the simultaneous determination of combinations of acetaminophen, phenylpropanolamine hydrochloride, guaifenesin, pseudoephedrine hydrochloride, caffeine, chlorpheniramine maleate, and dextromethorphan hydrobromide in cough and cold tablets and syrups. After extraction of the analyte with alkaline ethyl acetate, 2 microL extract was injected (splitting ratio of 50:1) into a gas chromatograph equipped with a CBP1-M25-025 fused silica capillary column (25 m x 0.22 mm; film thickness, 0.25 microm). The column temperature was held at 150 degrees C for 5 min, increased to 175 degrees C at 3 degrees C/min, and increased to 270 degreesC at 10 degrees C/min. The temperatures of the flame ionization detector and injector were maintained at 300 degrees C. The GC method is inexpensive, rapid, accurate, and precise, and thus it can be used for routine analysis of tablet and syrup preparations in quality control laboratories of pharmaceutical companies.     

固相萃取-毛细管气相色谱法测定中草药中13种有机氯农药的残留量

建立了中草药中有机氯类农药残留量的固相萃取-毛细管气相色谱(SPE-CGC)分析方法。对丹参、黄芩、射干、白芍、白芷、天南星、牛蒡子、知母、桔梗共9种中草药中六六六的4种异构体、滴滴涕的4种异构体、七氯、艾氏剂、环氧七氯、狄氏剂、异狄氏剂共13种有机氯农药的残留量进行了测定。以丙酮-正己烷混合物作提取剂,采用超声波提取样品,然后用Florisil固相萃取小柱快速净化提取物。采用SPB-5弹性石英毛细管气相色谱柱分离样品,电化学检测器进行检测。13种农药的峰面积与其质量浓度均有良好的线性关系,相关系数均大于0.998。最小检测量为0.064～0.61 μg/L;样品的加标回收率为87.3%～102.3%(相对标准偏差为1.3%～6.8%)。该法简便快速、灵敏准确,具有广泛的应用前景。     

Identification of hydrolyzed inulin syrup and high-fructose corn syrup in apple juice by capillary gas chromatography: PVM 4:1999

A peer-verified, gas chromatographic (GC) method is presented for the identification of hydrolyzed inulin syrup (HIS) and high-fructose corn syrup (HFCS) in apple juice. The procedure involves determining the Brix value of the apple juice or apple juice concentrate and preparing a dilution of the test sample to 5.5 degrees Brix. A 100 microL aliquot of the 5.5 degrees Brix test solution is then freeze-dried in a GC autosampler vial. The sugars in the freeze-dried residue are converted to trimethylsilyl derivatives, by the addition of an appropriate silylation reagent, and the vial is heated at 75 degrees C for 30 min. After derivatization, the solution is introduced into a gas chromatograph where the analytes are separated on a 30 m, 0.25 mm id DB-5 column. The method can use hydrogen, helium, or nitrogen as the carrier gas. The analytes and marker compounds are measured by use of a flame ionization detecone of the 2 syrups at 2 levels. Dilution was ascertained by the presence of retrograde sugar markers found in the 2 sugar syrups. All 3 laboratories involved in the study were able to identify the correct diluent in the blind, randomly coded, apple juice test portions. The levels of dilution in the test portions were 0, 6.9% (HIS), 16.0% (HIS), 8.1% (HFCS), and 17.0% (HFCS). No false positive results were reported. Quantitative conclusions can be drawn when the same syrup is used for dilution and as a reference standard.     

气相色谱法同时测定西草净、丁草胺和噁草灵

 采用气相色谱法,以癸二酸二正丁酯为内标物,对新研制的复合型稻田除草剂26％丁··西乳油进行了一次性定量分析。色谱条件为5％SE-302m×3mm的玻璃柱,柱温为210℃,检测温度为230℃。方法的回收率为98．62％～100．77％,线性相关系数大于0．999。方法准确、简便、快速。     

氯菊酯胺菊酯混合防蛀剂的气相色谱法测定

用３％ＯＶ－１０１２ｍ×３ｍｍｉ．ｄ．玻璃或不锈钢柱,以邻苯二甲酸二（２－乙基）己酯为内标,在柱温２２３℃时同时测定氯菊酯胺菊酯混合防蛀剂中有效成分——氯菊酯和胺菊酯的质量分数。方法中氯菊酯和胺菊酯的平均变异系数分别为０．２０％和０．１９％。     

气相色谱法检测大孔吸附树脂中的有机残留物

建立了同时检测大孔吸附树脂中苯、甲苯、二甲苯、苯乙烯、二乙苯、二乙烯苯、萘、癸烷、十一烷和十二烷等10种有机残留物的测定方法。以二氯甲烷为提取溶剂,采用超声提取法对样品进行前处理。采用气相色谱法检测,色谱柱为DB-624毛细管柱,检测器为氢火焰离子化检测器。上述10种有机残留物在12 min内能很好地分离,样品的加标回收率(n=3)为73.8%～107.9%,相对标准偏差为1.3%～4.4%,最低检测限为0.007～0.03 mg/L。本方法具有灵敏、准确、快速等特点。对9种商品树脂及其预处理品的有机残留物进行了测定,结果表明树脂预处理前后有机残留物的含量相差很大,经过预处理的树脂可以安全地应用于中药的生产。     

Enantioselective analysis of primaquine and its impurity quinocide by capillary electrophoresis

A capillary electrophoretic (CE) method for the baseline separation of the enantiomers of primaquine diphosphate (PQ) and quinocide (QC) (a major contaminant) in pharmaceutical formulations is proposed. Both components were separated under the following conditions: 50 mm tris phosphate buffer (pH 3.0) containing 15 mm hydroxypropyl-gamma-cyclodextrin (HP-gamma-CD) as background electrolyte; applied voltage, 16 kV; capillary temperature, 25 degrees C; detection wavelength, 254 nm; hydrostatic injection, 10 s. The separations were conducted using a 35 cm length and 50 microm i.d. uncoated fused silica capillary column. Under the optimized conditions, the components were successfully separated in about 5 min. Intraday precision of migration time and corrected peak areas when expressed as relative standard deviation ranged from 0.17 to 0.45 and 2.60 to 3.94%, respectively, while the interday precision ranged from 2.59 to 4.20 and 3.15 to 4.21%, respectively. After the validation exercise, the proposed method was applied for the determination of QC impurity in PQ formulations.     

界面衍生化气相色谱法测定葡萄酒中总有机酸

利用离子交换树脂分离、富集葡萄酒中总有机酸并直接在树脂界面上乙酯化,结合气相色谱／质谱法,鉴定并分析了葡萄酒中２１种有机酸。     

毛细管气相色谱法测定速效伤风胶囊中对乙酰氨基酚、咖啡因、马来酸氯苯那敏的含量

 用５％Ｐｈ－Ｍｅ－Ｓｉｌｉｃｏｎｅ毛细管色谱柱，ＦＩＤ，二阶程序升温，以正十六烷作为内标物测定速效伤风胶囊中对乙酰氨基酚、咖啡因、马来酸氯苯那敏的含量。浓度线性范围：对乙酰氨基酚４～２０ｇ／Ｌ，咖啡因０．０８４～０．４２ｇ／Ｌ，马来酸氯苯那敏０．１５～０．７５ｇ／Ｌ。平均回收率（ｎ＝５）：对乙酰氨基酚９９．６２％（ＲＳＤ＝０．４４％）咖啡因９６．４６％（ＲＳＤ＝１．３２％），马来酸氯苯那敏９８．５５％（ＲＳＤ＝０．６５％）。     

气相色谱法快速测定家用气雾杀虫剂中丙烯菊酯、氯菊酯、增效醚含量

用气相色谱法定量测定了家用气雾杀虫剂中的丙烯菊酯、氯菊酯和增效醚。色谱柱为５％ＱＦ－１／Ｃｈｒｏ－ｍｏｓｏｒｂＷＨＰ,以邻苯二甲酸二苯酯为内标物,测得的回收率分别为１００％,１０２％,９９．９％;变异系数为０．１３,０．５６,０．４８,方法简便、快速、准确。     

大口径毛细管气相色谱法测定罂粟壳中的生物碱

摘要：采用超声提取大口径毛细管气相色谱法同时测定罂粟壳中可待因、吗啡、蒂巴因、罂粟碱和那可汀的质量比,用HP-1（5m×0.53mm×2.65μm）毛细管柱,GC-FID测定,结果表明,可待因、吗啡、蒂巴因、罂粟碱和那可汀的平均回收率分别为94.0％,96.5％,93.8％,91.0％,91.4％,RSD=0.92％～2.75％。     

固相萃取-气相色谱-质谱法测定利多卡因代谢物单乙基甘氨酰二甲苯胺的血药浓度

建立了固相萃取-气相色谱-质谱(GC-MS)测定利多卡因代谢物单乙基甘氨酰二甲苯胺(MEGX)血药浓度的方法。血清中的MEGX采用固相萃取小柱萃取、GC-MS测定。色谱条件为：HP-5MS毛细管柱(15 m×0.25 mm×0.1 μm),初始柱温100 ℃,保持1 min后以40 ℃/min速率升温至200 ℃,保持0.5 min;进样口温度250 ℃;分流进样,分流比1∶1,进样量2 μL;载气为氦气,流量为1.0 mL/min。质谱条件为:离子源温度230 ℃,电子轰击电离,电子能量70 eV,选择离子检测（m/z 58(MEGX)、 m/z 86(普鲁卡因,内标)）。结果表明,MEGX在血清中的浓度在1.562～25 ng/mL范围内的线性关系良好,相关系数0.9981,最低检测限为0.5 ng/mL,不同浓度MEGX的萃取回收率在80.1%～85.7%之间。实验证明该方法快速、准确,选择性好,灵敏度高,适合用于血清中微量MEGX的测定。     

气相色谱-质谱法测定大蒜挥发油的组成

采用改进的水蒸汽蒸馏法从山东金乡大蒜中提取挥发油。实验确定了气相色谱-质谱法分析大蒜油的条件,并对大蒜挥发油的化学成分进行了定性分析,共鉴定出20种物质。用峰面积归一化法对各物质的相对含量进行了测定,结果表明含硫化合物约占挥发油总成分的95%以上,其中含量最高的是大蒜新素,约占挥发油总量的三分之一。对低温储藏半年的挥发油进行分析的结果表明样品在低温下可稳定存放。     

A rapid and simple high-performance liquid chromatography method for the determination of human plasma levofloxacin concentration and its application to bioequivalence studies

A high-performance liquid chromatography method with fluorescence detection (HPLC-FLD) for the determination of levofloxacin in human plasma is described. Neutralized with phosphate buffer (pH 7.0), the sample (0.1 mL) was extracted with dichlormethane (1 mL). After voltex-mixing and centrifuged at 3000g for 6 min at 4 degrees C, the upper aqueous layer was aspirated using a micro vacuum pump and the organic layer was directly transferred to a clean test tube without pipetting. The organic solvent was evaporated and the residues were reconstituted with the mobile phase. Levofloxacin and terazosin (internal standard, IS) were chromatographically separated on a C(18) column with a mobile phase containing phosphate buffer (pH 3.0, 10 mm), acetonitrile and triethylamine (76:24:0.076, v/v/v) at a flow rate of 1 mL/min. The analytes were detected using fluorescence detection at an excitation and emission wavelength of 295 and 440 nm, respectively. The linear range of the calibration curves was 0.0521-5.213 microg/mL for levofloxacin with a lower limit of quantitation (0.0521 microg/mL). The retention times of levofloxacin and terazosin were 2.5 and 3.1 min, respectively. Within- and between-run precision was less than 12 and 11%, respectively. Accuracy ranged from -6.3 to 4.5%. The recovery ranged from 86 to 89% at the concentrations of 0.0521, 0.5213 and 5.213 microg/mL. The present HPLC-FLD method is sensitive, efficient and reliable. The method described herein has been successfully used for the pharmacokinetic and bioequivalence studies of a levofloxacin formulation product after oral administration to healthy Chinese volunteers.     

应用搅拌棒吸附萃取-热脱附-气相色谱-质谱测定烟叶和茶叶中拟除虫菊酯类农药残留

应用搅拌棒吸附萃取(SBSE)技术分别萃取烟叶和茶叶中的5种拟除虫菊酯,并利用热脱附系统将萃取到的物质进行热脱附,然后通过气相色谱-质谱联用仪(GC-MS)进行分析测定。实验过程中对影响SBSE的因素及影响热脱附的条件进行了优化。在优化条件下,采用外标法分别对烟叶和茶叶中的5种拟除虫菊酯类农药残留进行了定量分析。结果表明,烟叶中5种拟除虫菊酯的检出限范围为3.3~11.4 ng,加标回收率为94.8%~103.4%,6次测定的相对标准偏差（RSD）为5.3%~8.6%;茶叶中5种拟除虫菊酯的检出限范围为4.2~10.5 ng,加标回收率为98.2%~110.1%,6次测定的RSD为5.0%~9.6%。实验证明该法具有较高的准确度、灵敏度和较好的重现性,可用于烟叶和茶叶中拟除虫菊酯类农药残留的快速分析测定。     

高效液相色谱法同时测定烟用甘草提取物中14种活性成分

0.100 0g的甘草提取物样品用10mL的80%(体积分数)甲醇溶液超声提取30min后静置30min,取上清液经0.45μm滤膜过滤。采用高效液相色谱法同时测定滤液中14种活性成分的含量,以Diamonsil Plus C18色谱柱为分离柱,用0.05%(体积分数)磷酸溶液和乙腈以不同比例混合的溶液为流动相进行梯度洗脱,用二极管阵列检测器测定。通过单因素试验和L9(33)正交试验对提取条件进行了优化。14种活性成分的质量浓度在一定范围内与其对应的峰面积呈线性关系,方法的检出限(3s)为0.02~0.12 mg·L^-1。在3个浓度水平进行加标回收试验,回收率为91.7%~143%,测定值的相对标准偏差(n=5)为1.2%~6.0%。     

An efficient immunoaffinity chromatographic method for extraction and purification of papaverine from samples of pericarpium papaveris and food products

A highly selective immunoaffinity column was obtained by coupling anti-papaverine polyclonal antibodies to CNBr-activated Sepharose 4B. It was found that the coupling efficiency and performance of the immunoaffinity column were greatly improved by prolonging the coupling reaction time from 3 h at 20 degrees C with shaking to incubation overnight at 4 degrees C after the 3 h shaking reaction. The pH and ionic strength were observed to be the most important factors that influence the binding of papaverine to the immunoaffinity column. Using 0.01 mol/L phosphate buffered saline (PBS, pH 8.3) and methanol-water (80:20, v/v) as the loading and eluting solutions, respectively, papaverine was first retained on the column and then quantitatively eluted out with a mean recovery of 86% at a loading concentration of 1 microg/mL. When applied to real samples of pericarpium papaveris and food products, the established immunoaffinity column showed high efficiency in removing the matrix interferences in the samples and satisfactory recovery results were obtained. The method was useful for extraction and purification of papaverine from related samples.