高效液相色谱法同时检测牙膏中19种合成着色剂

建立了高效液相色谱法(HPLC)同时测定牙膏中19种合成着色剂的检测方法.样品经水分散后超声提取,以10000 r/min离心5min,经0.45μm微孔聚四氟乙烯(PTFE)过滤后取滤液测定.采用Agilent eclipse XDB-C18柱(4.6 mm×150 mm,5μm),以乙腈和20 mmol/L乙酸铵溶...     

超高效液相色谱法测定纺织品中三氯生的含量

建立了快速准确测定纺织品中三氯生含量的高效液相色谱法,该方法以二氯甲烷为提取溶剂,超声提取了纺织品中的抗菌剂三氯生,提取液经浓缩吹干后用流动相定容,以甲醇-水(90∶10)为流动相,采用二极管阵列(PDA)检测器进行检测。该方法的线性范围为0.5~80 mg/L,检出限(S/N=3)为0.1 mg/L,回收率为95%~105%。     

高效液相色谱法测定洗涤用品中三氯生和三氯卡班

建立了同时测定洗涤用品中三氯生和三氯卡班的高效液相色谱法。液、皂、粉3类洗涤用品先经甲醇超声提取离心后用高效液相色谱法测定。采用C8色谱柱,甲醇/水梯度洗脱,检测波长281 nm,二者得到良好分离。三氯生在0.5~100 mg/L范围内(r2=0.999),三氯卡班在0.1~100 mg/L范围内(r2=0.999)线性关系良好;方法定量限分别为0.0025%和0.0005%。低、中、高3个添加水平的回收率在96.3%~109.5%,相对标准偏差为0.3%~7.3%(n=6)。采用本方法对24件市售洗涤用品进行抽查,其中5件液类样品检出三氯生,2件皂类样品检出三氯卡班。     

高效液相色谱法测定游泳池水中三氯卡班、三氯生和甲基三氯生的含量

采用高效液相色谱法测定游泳池水中三氯卡班、三氯生和甲基三氯生的含量。样品经HLB固相萃取柱(200mg,6mL)富集,净化,采用PICKERING-C8色谱柱(4.6mm×250 mm,5μm)分离,以甲醇-水溶液为流动相进行梯度洗脱,在检测波长281nm处进行测定。三氯卡班、三氯生和甲基三氯生的质量浓度均在0.025~10mg·L^-1内与其峰面积之间呈线性关系,方法的检出限(3S/N)为0.007 5~0.015 mg·L^-1。按标准加入法进行回收试验,测得加标回收率为91.4%~104%,相对标准偏差(n=6)为2.5%~9.3%。     

高效液相色谱法同时测定牙膏及漱口水中的23种致癌染料

建立了同时测定牙膏和漱口水中23种致癌染料的高效液相色谱(HPLC)检测方法.漱口水样品直接以乙醇溶解稀释,牙膏样品烘干后以乙醇超声提取.采用ZORBAX Eclipse XDB-Phenyl(150 mum x 4.6 mm x 5 pm)色谱柱进行分离,以2.5 mmol/L磷酸二氢四丁基铵水溶液(pH7.5)和甲...     

超高效液相色谱法同时测定牙膏中5种植物源活性成分

建立了同时测定牙膏中丹皮酚(Pae)、麝香草酚(Thy)、和厚朴酚(Hon)、厚朴酚(Mag)、甘草次酸(Gly)5种植物源活性成分的超高效液相色谱方法。牙膏样品以90%甲醇为溶剂超声提取,离心取上清液过滤后进行分析,采用Waters ACQUITY UPLCHSS C_(18)(2. 1 mm×100 mm,1. 8μm)为分离柱,乙腈-0. 1%甲酸(pH 2. 8)为流动相,梯度洗脱,流速为0. 3 mL/min,二极管阵列检测器(PDA)的检测波长为275、250nm,外标法定量。结果表明,5种植物源活性成分在2～100 mg/L质量浓度范围内呈良好的线性关系,相关系数(r)均大于0. 999;检出限为0. 2～1. 0 mg/kg,定量下限为0. 8～3. 5 mg/kg;在4个加标水平下的平均回收率为90. 5%～99. 4%,相对标准偏差(RSD)为0. 7%～5. 1%。该法分析快速、重复性好、准确性好、灵敏度高,已应用于实际牙膏样品的测定。     

高效液相色谱法检测水体中微囊藻毒素

建立了高效液相色谱检测水体中微囊藻毒素(Microcystins,MCs)的方法.选择XAD-2树脂为富集树脂,采用四氯化碳-10%乙醇-10%丙酮连续淋洗,获得较好的杂质去除效果,采用90%甲醇可以将树脂柱上的MCs完全洗脱.HPLC采用V(0.1% TFA):V(甲醇)=42: 58混合溶液为流动相进行等度洗脱,MC-RR和 MC-LR取得较好分离效果,回收率均达到90%以上.水样富集2000倍后,方法的检出限为0.05 μg/L.本方法操作简便、灵敏度高、检测速度快.     

反相高效液相色谱法测定牙膏中的甘草次酸

采用反相高效液相色谱法测定了牙膏中的甘草次酸。在ＹＷＧ Ｃ１８（４０ｍｍｉ．ｄ．×２５０ｍｍ,１０μｍ）色谱柱上,以Ｖ（甲醇）∶Ｖ（００１ｍｏｌ／ＬＫＨ２ＰＯ４）＝８５∶１５（ｐＨ３０）的溶液为流动相,流速为１０ｍＬ／ｍｉｎ,紫外检测波长为２５４ｎｍ,室温下检测。甘草次酸用甲醇提取。甘草次酸的平均回收率为９９６１％～１０１６７％,样品测试相对标准偏差为１８５％～３１６％。方法操作简便、快速和准确。     

固相萃取-高效液相色谱法测定牙膏中黄芩甙

建立了固相萃取-高效液相色谱法(HPLC)检测牙膏中黄芩甙的分析方法。样品用75%乙醇超声提取20min,8 000r/min离心10min,取5mL上清液经MAX固相萃取柱处理,5%甲酸-甲醇溶液洗脱后氮吹浓缩后分析。采用ZORBAX SB C18色谱柱;流动相为乙腈-0.1%磷酸(体积比22∶78),检测波长为276nm。该方法线性范围1～100μg·mL-1,加标回收率81.3%～101.6%,检出限3.0mg·kg-1。方法准确、重现性好,干扰能力强,适用于牙膏中黄芩甙的检测。     

高效液相色谱法测定硫酸沙丁胺醇

利用高效液相色谱仪-电子捕获检测器(HPLC-ECD)测定了市售片剂硫酸沙丁胺醇的含量.结果表明,利用HPLC-ECD技术测定硫酸沙丁胺醇的线性范围为0.944~33.8mg·L-1(r=0.999 6);回收率为99.0%~107.8%(RSD≤4.6%).该法可用于测定片剂的硫酸沙丁胺含量.     

Determination of forsythiaside in rat plasma by high-performance liquid chromatography and its application to pharmacokinetic studies

A simple high-performance liquid chromatographic method was developed to study the pharmacokinetics of forsythiaside in rat plasma after intravenous administration. Hesperidin was used as the internal standard. The drugs were separated on a reversed-phase C(18) column and detected at 332 nm. Good linearity was achieved in the range of 0.067-26.667 microg/mL. The intra- and inter-assay variation coefficients for this analysis were no more than 10.94 and 14.56%, respectively. The average recovery for forsythiaside was 87.42% from plasma. The analytical sensitivity and accuracy of this assay were adequate for characterization of the pharmacokinetics of intravenous administration of forsythiaside to rats and the assay has been successfully applied to provide pharmacokinetic data. The mean t(1/2Z) was 20.36, 19.40 and 23.62 min for 2, 5 and 20 mg/kg for forsythiaside after i.v. administration, respectively. The AUC(0-t) increased linearly from 40.64 to 624.14 microg min/mL after administration of the three doses.     

Determination of methoxsalen in dosage forms by high-performance liquid chromatography

Summary A new, rapid, sensitive, and specific method for the determination of methoxsalen in dosage forms using HPLC has been developed. methoxsalen is extracted in chloroform, evaporated on a water bath, and the residue is redissolved in ethanol. A standard solution of khellin (internal standard) in ethanol is added, and injected. A plot of peak height ratio (methoxsalen/internal standard) vs. concentration of methoxsalen gave a straight line (r=0.998). The column used was a stainless steel, 3.8 mm×30 cm, and the mobile phase was methanol: water (6040) at a flow rate of 2 cm³/min. Retention times for methoxsalen and khellin were 3.45 and 9.6 min, respectively. This method was found superior to the spectrophotometric assay in that no interference was encountered from structurally similar compounds or from coloring agents used in some commercial methoxsalen products.     

高效液相色谱法同时检测8种喹诺酮类兽药残留量

建立了吡哌酸、氧氟沙星、环丙沙星、单诺沙星、恩诺沙星、沙拉沙星、(噁)喹酸和氟甲喹8种喹诺酮类兽药残留量的高效液相色谱-荧光检测方法. 方法的线性范围: 30～2000 μg/kg, 定量限为30 μg/kg, 检出限为5 μg/kg (吡哌酸为20 μg/kg). 该方法采用基质分散和微波萃取技术进行样品的前处理, 回收率为70.0%～99.5%, 相对标准偏差1.0%～8.5%. 并同固相萃取方法进行了比较, 分别使用了RPS、HLB、MAX 3种固相萃取柱, 其回收率均低于本法. 确立了以Aglient XDB-C18 (5 μm, 150 mm×4.6mm i.d.)色谱柱, H3PO4-纯水-三乙胺-乙腈(pH 3.0)为流动相的最佳色谱条件, 吡哌酸、氧氟沙星、环丙沙星、单诺沙星、恩诺沙星、沙拉沙星的检测波长为: 激发波长285 nm, 发射波长460 nm;(噁)喹酸和氟甲喹为: 激发波长325 nm, 发射波长365 nm. 方法可满足兽药残留检测要求.     

高效液相色谱法测定粮食制品中甲醛残留量

研究建立了一种用HPLC测定粮食制品中甲醛残留量的分析方法。样品中甲醛经60℃水浴提取,与2,4 二硝基苯肼衍生后,生成的2,4 二硝基苯腙经石油醚萃取净化,用HPLC DAD分离测定,外标法定量。最小检出质量浓度为5×10-11g,对于5g样品,最低检出量为0.01mg kg,样品回收率>80%,相对标准偏差≤10%,能满足残留量分析的要求。     

Determination of polyamines by high-performance liquid chromatography with chemiluminescence detection

A method was developed for the determination of polyamines (PA) by high-performance liquid chromatography with chemiluminescence detection. It is based on the unsaturated complex of PA with Cu(II) which had a strong catalytic effect on the luminol-H₂O₂ chemiluminescence reaction. The separation of PA was carried out on a reveres phase C18 column using methanol/water (25/75, v/v) as a mobile phase. The method was applied to the analysis of putrescine and the total amount of spermine and spermidine in apple leaves and strawberry fruit. The results indicated that the method is practical and useful.     

Determination of atractylenolide II in rat plasma by reversed-phase high-performance liquid chromatography

A method for quantitative determination of atractylenolide II in rat plasma using reversed-phase high-performance liquid chromatography (RP-HPLC) coupled with UV spectrometry was established. From a variety of compounds and solvents tested, atractylenolide III was selected as the internal standard (IS) and ethyl acetate was found to be the best solvent for extracting atractylenolide II from plasma samples. RP-HPLC analysis of the extracts was performed on an analytical column (DIKMA ODS, 150 x 4.6 mm; i.d., 5 microm) equipped with a security guard pre-column system. There was good linearity over the range 0.05-5.0 microg/mL (r > 0.99). The recoveries were more than 90.0% in plasma, and the intra- and inter-day coefficients of variation were less than 10.0% in all cases. The limit of detection (LOD) was 0.025 microg/mL and the lower limit of quantification (LLOQ) was 0.05 microg/mL. The RP-HPLC method was applied to quantitate atractylenolide II in rat plasma within 24 h in a pharmacokinetics study where experimental rats received a single dose of atractylenolide II (60 mg/kg).     

Determination of diclofenac in plasma by high-performance liquid chromatography with electrochemical detection

A reversed-phase high-performance liquid chromatographic method with electrochemical detection for the quantitative determination of diclofenac potassium in plasma was developed. Naproxen was used as the internal standard. The drug and internal standard were isolated from plasma by extraction with dichloromethane and 2 M hydrochloric acid. Chromatographic separation was performed on a C18 column with methanol-water (68:32, v/v) adjusted to pH 3.2 with phosphoric acid as mobile phase. The oxidation potential for detection was established by constructing a voltammogram for diclofenac. The quantification limit for diclofenac in plasma was 5 ng mL(-1). Linearity of the method was confirmed in the range 5-2000 ng mL(-1), correlation coefficient 0.9998. Within-day relative standard deviations (RSDs) ranged from 0.66 to 14.00% and between-day RSDs from 0.59 to 15.78%. The method was successfully applied for the determination of pharmacokinetic parameters after ingestion of a 50 mg dose of diclofenac. Studies were performed on 18 healthy volunteers of both sexes.     

Chemical fingerprint analysis of Fritillaria delavayi Franch. by high-performance liquid chromatography

Bulbus of Fritillaria delavayi Franch. is the most commonly used antitussive and apophlegmatic in China and commonly prepared by water decoction. In this study, a novel and reliable method of high-performance liquid chromatography (HPLC) was developed both for quantitative analysis of 10 bioactive compounds (uracil, cytidine, inosine, uridine, guanosine, thymidine, adenosine, hypoxanthine, adenine and 2-deoxyadenosine) and chemical fingerprint analysis of F. delavayi Franch. In quantitative analysis, 10 compounds showed good regressions (R(2) > 0.9982) within test ranges and the recovery of the method was in the range of 96.33-104.51%. In the fingerprint analysis, 11 characteristic peaks were selected to evaluate the similarities of F. delavayi Franch. samples, and the HPLC chromatograms of 16 samples from different regions of China showed similar patterns. The results from the experiment demonstrated that the combinations of the quantitative and chromatographic fingerprint analysis offer an efficient way to evaluate the quality consistency of F. delavayi Franch.     

Determination of tetracyclines residues in honey by on-line solid-phase extraction high-performance liquid chromatography

An automated system using on-line solid-phase extraction (SPE) high-performance liquid chromatography (HPLC) with ultraviolet (UV) detection was developed for the determination of tetracyclines (TCs), such as tetracycline (TC), oxytetracycline (OTC), chlortetracycline (CTC), metacycline (MC), and doxycycline (DC) in honey. One milliliter diluted honey sample was injected into a conditioned C18 SPE column and the matrix was washed out with water for 3 min. By rotation of the switching valve, TCs were eluted and transferred to the analytical column by the chromatographic mobile phase. Chromatographic conditions were optimized. TCs were separated in less than 8 min with a gradient elution using a mixture of 0.8% formic acid and acetonitrile. The UV detection was performed at 365 nm. The conditions for on-line SPE, including solvent and total time for loading sample and washing matrix were also optimized. Time for extraction and separation decreased greatly. For the five kinds of TCs, the limits of detection (LODs) at a signal-to-noise of 3 ranged from 5 to 12 ng g⁻¹. The relative standard deviations (R.S.D.) for the determination of TCs ranged from 3.4 to 7.1% within a day and ranged from 3.2 to 8.9% in 3 days, respectively.