Imidazolium ionic liquid as the background ultraviolet absorption reagent for determination of morpholinium cations by high performance liquid chromatography-indirect ultraviolet detection

A novel analytical method was developed for determining morpholinium cations lacking ultraviolet absorption groups.This determination was carried out by high performance liquid chromatographyindirect ultraviolet（HPLC-1UV） detection using imidazolium ionic liquid as background absorption reagents,and imidazolium ionic liquid aq.soln.-organic solvent as mobile phase by a reversed-phase C18 column.The background ultraviolet absorption reagents,imidazolium ionic liquids and organic solvents were investigated.The imidazolium ionic liquid in the mobile phase is not only the background ultraviolet absorption reagent for IUV,but also an active component to improve the separation of morpholinium cations.It was found that morpholinium cations could be adequately determined when0.5 mmol/L 1-ethyl-3-methylimidazolium tetrafluoroborate aq.soln./methanol（80：20,v/v） was used as mobile phase with an IUV detection wavelength of 210 nm.In this study,the baseline separation of Nmethyl,ethylmorpholinium cations（MEMo） and N-methyl.propylmorpholinium cations（MPMo） was successfully achieved in 8.5 min.The detection limits（S/N = 3） for MEMo and MPMo were 0.15 and0.29 mg/L,respectively.This simple and practical method has been successfully applied to the determination of two morpholinium ionic liquids synthesized by the chemistry laboratory.

Trace Determination of Tamoxifen in Biological Fluids Using Hollow Fiber Liquid-Phase Microextraction Followed by High-Performance Liquid Chromatography-Ultraviolet Detection

The applicability of hollow fiber liquid-phase microextraction (HF-LPME) combined with high-performance liquid chromatography-ultraviolet detection (HPLC-UV) was evaluated for the extraction and determination of tamoxifen (TAM) in biological fluids including human urine and plasma. The drug was extracted from a 15 mL aqueous sample (source phase;SP) into an organic phase impregnated in the pores of the hollow fiber (membrane phase;MP) followed by the back-extraction into a second aqueous solution (receiving phase;RP) located in the lumen of the hollow fiber. The effects of several factors such as the nature of organic solvent, compositions of SP and RP solutions, extraction time, ionic strength and stirring rate on the extraction efficiency were examined and optimized. An enrichment factor of 360 along with substantial sample clean up was obtained under the optimized conditions. The calibration curve showed linearity in the range of 1 - 500 ng?mL–1 and the limit of detection was found to be 0.5 ng?mL–1 in aqueous medium. A reasonable relative recovery (≥89%) and satisfactory intra-assay (3.7% - 4.2%, n = 3) and inter-assay (7.5% - 7.8%, n = 3) precision illustrated good performance of the analytical procedure in spiked human urine and plasma samples.

Separation and identification of moxifloxacin impurities in drug substance by high-performance liquid chromatography coupled with ultraviolet detection and Fourier transform ion cyclotron resonance mass spectrometry

In this paper, a high-performance liquid chromatography coupled with ultraviolet detection and Fourier transform-ion cyclotron resonance mass spectrometry （HPLC-UV/FrICRMS） method was described for the investigation of impurity profile in moxifloxacin （MOX） drug substance and chemical reference substance. Ten impurities were detected by HPLC-UV, while eight impurities were identified by using the high accurate molecular mass combined with multiple-stage mass spectrometric data and fragmentation rules. In addition, to our knowledge, five impurities were founded for the first time in MOX drug substance.

高效液相色谱-紫外检测法同时测定类鼻疽患者血浆中亚胺培南、美罗培南和头孢他啶的浓度

目的建立一种快速、经济的高效液相色谱-紫外检测法(HPLC-UV),用于同时测定人血浆中亚胺培南、美罗培南和头孢他啶的药物浓度。方法采用Millipore 10KD超滤离心去蛋白,使用互为内标法,色谱柱为SunFire-C18柱(4.6 mm×250 mm,5µm);预柱为C18柱(4.0 mm×2.1 mm,5µm),流动相为0.1 mol·L^(-1)的3-(N-吗啡啉)丙磺酸(pH=7.0)和乙腈,梯度洗脱,检测波长299nm,流速1.0mL·min^(-1),运行时间30min,进样体积30µL。结果亚胺培南、美罗培南和头孢他啶的保留时间分别为6.699 min、10.795 min和8.722 min。血浆内源性物质对样品的测定无干扰,峰形良好。该方法具有良好的线性、准确度和精密度。不同浓度的样品在–20℃反复冻融、–20℃长期冷冻和4℃(48 h)下均表现出了较高的稳定性。结论该方法操作成本低、专属性强、分离效果好,可用于类鼻疽患者血浆中亚胺培南、美罗培南和头孢他啶治疗药物浓度的测定。

大蒜辣素软膏的体外透皮吸收特性研究

目的研究大蒜辣素软膏在离体大鼠皮肤的吸收特性。方法通过Franz扩散池,建立离体大鼠完整背部皮肤及去角质层皮肤的透皮模型,采用超高效液相色谱-质谱-质谱串联法(UPLC-MS-MS)测定大蒜辣素软膏透皮吸收液中大蒜辣素的含量,测定大蒜辣素软膏的体外透皮吸收特性,并评价该大蒜辣素累积透过量及渗透速率。结果大蒜辣素5 h内体外经皮渗透量Q与时间t线性关系较好,均符合Higuchi动力学过程,回归相关系数(r)均达到0.99以上。完整皮肤的透皮速率J为12.306μg·cm^(-2)·h^(-1),去角质层皮肤的J为58.353μg·cm^(-2)·h^(-1),去角质层皮肤的J高于完整皮肤。结论大蒜辣素软膏有效成分可经皮渗透,主要以原型形式吸收,角质层厚度是影响大蒜辣素软膏透过皮肤的重要因素。

高效液相色谱-紫外检测法测定化妆品中咖啡因的含量

建立了高效液相色谱法测定化妆品中咖啡因的含量。试样经甲醇提取稀释后或正己烷分散再用甲醇水溶液反萃提取净化后,采用Waters Atlantis T3色谱柱(4.6 mm×150 mm,5μm)分离,以甲醇和水为流动相梯度洗脱,流速为1.0 mL/min,检测波长为273 nm,柱温为40℃。结果表明,咖啡因在0.2~10 mg/kg的质量浓度范围内呈现良好线性关系,相关系数为0.9999,七种基质三个浓度水平的平均回收率在105.5%~110%之间,RSD在0.7%~4.5%之间,方法的定量限为10 mg/kg。建立的方法具有提取效率高、分析时间短、测试结果准确可靠、重复性好等优点,可适用于化妆品中咖啡因的含量测定。

紫外可见-光谱库在农药除草剂隐性成分排查中的应用

通过高效液相色谱法,建立了113种常规除草剂的标准紫外-可见光谱图库,检测除草剂中的隐性成分。以乙腈磷酸水为流动相的梯度洗脱对除草剂隐性成分进行定性分析。通过光谱库对2个农药除草剂进行了隐性成分鉴定,检出了敌稗、噁唑酰草胺和2甲4氯3种隐性成分。此方法能够快速准确的查出除草剂中添加的隐性成分,特征性和专属性很强,能够克服保留时间定性时容易造成假阳性的结果;该方法操作简单、检测效率高、时间短和成本低,适合于农药分析人员。

不同产地滇黄精高效液相色谱法指纹图谱的建立及其多糖含量测定

目的探讨不同产地滇黄精高效液相色谱法(HPLC)指纹图谱的建立及其多糖含量的测定。方法取贵州(剑河、安顺、天柱、铜仁、赤水、贵阳及纳雍)、广西百色及四川内江来源的9个批次滇黄精药材各1 g制备供试品溶液,采用DiKMA Platisll ODS C_(18)色谱柱(流动相为乙腈-0.05%磷酸水溶液、梯度洗脱,流速1 mL/min,柱温35℃,进样量20μL,检测波长203 nm)建立滇黄精HPLC指纹图谱,并采用相似度评价、主成分分析及聚类分析等方法评价不同产地滇黄精的质量;采用蒽酮-硫酸法测定各批次滇黄精的多糖含量。结果建立了9批滇黄精的HPLC指纹图谱,共确认12个共有峰;9批不同产地的滇黄精多糖含量均大于7%,含量顺序为贵州剑河>贵州安顺>贵州天柱>贵州铜仁>贵州赤水>贵州贵阳>贵州纳雍>广西百色>四川内江;相似度结果显示,四川内江、贵州贵阳及广西百色的相似度分别为0.762、0.809及0.846,贵州其余地区滇黄精的相似度≥0.853;主成分分析结果显示共得到3个主成分因子,聚类分析结果表明滇黄精被分为3类,且滇黄精多糖含量≥7.16%。结论本研究建立的滇黄精HPLC指纹图谱及黄精多糖成分含量的测定方法简便可行,准确可靠。

药用辅料乳糖中痕量亚硝酸盐和硝酸盐的离子色谱-电导/紫外检测研究

目的:建立药用辅料乳糖中痕量亚硝酸盐、硝酸盐的离子色谱-抑制电导(IC-CD)检测法和高效液相色谱-紫外(HPLC-UV)检测法。搭建在线膜抑制系统,结合LC-MS/MS技术进行结构确证,为药用辅料乳糖的前置风险控制提供新的策略。方法:IC-CD检测法和HPLC-UV检测法均采用高容量阴离子交换柱Dionex IonPacTM AS11-HC RFICTM(4.0 mm×250 mm)和保护柱Dionex IonPacTM AS11-HC RFICTM(4.0 mm×50 mm)。IC-CD检测法流动相为氢氧化钾溶液,梯度洗脱,抑制型电导检测器的电导池温度为30℃;HPLC-UV检测法流动相为5 mmol·L^(-1)氢氧化钠溶液,检测波长为210 nm;两种方法的流速均为1.0 mL·min^(-1),柱温均为30℃,进样量均为25μL。结果:两种方法测定亚硝酸根在0.03~10μg·mL^(-1)范围内、硝酸根在0.02~200μg·mL^(-1)范围内线性关系均为良好(r>0.999);亚硝酸根检测限和定量限分别为0.25 ng和0.75 ng,硝酸根检测限和定量限分别为0.25 ng和0.50 ng;回收率在84.00%~100.70%之间;进样精密度RSD(n=6)在0.27%~1.33%之间;均满足检验需求。结论:两种方法均具有灵敏度高、专属性强、分离度好、前处理简单的优势,可表征药用辅料乳糖中痕量亚硝酸盐、硝酸盐的含量,也为其他药用辅料前置风险研究提供新的思路和参考。

克林霉素甲硝唑搽剂原料甲硝唑供应商变更质量研究

目的:克林霉素甲硝唑搽剂变更原料甲硝唑供应商,为评估原料供应商变更对制剂质量的影响,对变更前后供应商原料甲硝唑进行质量对比研究;对变更前后制剂杂质进行对比研究;对变更前后制剂产品进行质量稳定性研究。方法:采用粉末X射线衍射法、激光粒度分析法、高效液相色谱法,对原料甲硝唑进行晶型、粒度分布、杂质、含量对比研究,对制剂产品进行杂质及质量对比研究,开展稳定性试验研究。结果:变更前后供应商原料甲硝唑质量对比,为同一晶型原料药,粒度分布基本一致,杂质及含量无明显差异;甲硝唑变更前后制剂杂质及质量对比无明显差异;甲硝唑变更前后生产产品经稳定性对比试验,各项检测结果均无明显变化,质量稳定。结论:变更原料甲硝唑供应商,原料甲硝唑质量无明显差异,未对产品质量产生不良影响。

药品检验中的结果偏离原因及质量控制方法研究

目的:探究药品检验中的结果偏离原因及质量控制方法。方法:择取江西领行生物科技有限公司药物样本200份(2022年1月-2022年12月)进行研究,均采用紫外分光光度法、高效液相色谱法检验,分析偏离原因与质控方法。结果:质量控制前,偏离原因受操作、仪器、实验室污染、检验差错的影响,质控后,仅出现实验室污染、检验差错偏离。结论:药品检验时,选择有效检验方法可提升检验准确度。

高效液相色谱法测定香附中α-香附酮的含量

目的通过高效液相色谱法(High Performance Liquid Chromatography,HPLC)探索香附中α-香附酮的提取方式和含量的测定方法,达到方法准确可靠简便易操作的目的。方法采用高效液相色谱法。色谱柱为Agilent Eclipse Plus,十八烷基硅烷键合硅胶色谱柱,150×4.6 mm,5μm,流动相为:甲醇—水(70:30),紫外-可见分光检测器;流速为1.0 mL/min;检测波长为240 nm;柱温为35℃。结果香附在0.02314-0.46287 mg/mL线性范围内呈良好线性关系,R2=1,平均回收率99.84%,RSD(Relative Standard Deviation)=0.09%。结论该方法操作简便,灵敏度高,重复性好,准确、可靠,可用于测定香附α-香附酮的含量,并有效控制香附的质量。

重金属检测技术在水质分析中的应用

水质污染是当前环境领域的一大难题,尤其是由于工业化和城市化进程的加速,重金属污染引起了广泛关注。为了有效监测和控制水中重金属的浓度,各种先进的检测技术应运而生。本文首先介绍了水质中重金属常见的检测方法,如原子吸收光谱和荧光光谱,然后重点关注了近年来涌现的新型技术,包括电化学检测技术和生物检测技术。这些新技术不仅具有高灵敏度和选择性,而且具有实时监测和迅速响应的优势。

阿司匹林含量测定方法研究进展

阿司匹林为临床常用药品,因其确切的疗效和较小的药物不良反应而为大众所熟知,根据近年来阿司匹林含量测定方法研究成果,介绍滴定法、紫外-可见分光光度法、高效液相色谱法、近红外漫反射法等在测定阿司匹林含量方面的研究进展,为进一步开发阿司匹林新的检测方法提供参考依据。

Qualitative Analysis of Xinyue Capsules(心悦胶囊)by High-Performance Liquid Chromatography:Preliminary Evaluation of Drug Quality in A Sino-Austrian Joint Study

ABSTRACT Objective： To develop a reliable method to assess the stability of Xinyue Capsules （心悦胶囊） containing Panax quinquefolius saponins according to European quality standards. Methods： An efficient high-performance liquid chromatography ultraviolet （HPLC-UV） method was established to analyse six main ginsenosides （Rb1, Rb2, Rc, Rd, Re and Rg1） in six different batches （120 capsules/batch） from the same lot of Xinyue Capsules and in one batch measured six times within one day. The six ginsenosides were separated on a Hypersil BDS-C18 column （3 μm, 100 mm × 3 mm） at a flow rate of 0.5 mL/min. Gradient elution was performed using a mobile phase gradient of acetonitrile-water modified with 0.01% formic acid. The HPLC chromatograms were analyzed with ＂LC data comparison＂ using Lab Solutions software. Results： The HPLC peaks were identified by comparing their retention times （Rg1： 23.44 min, Re： 23.77 rain, Rb1： 35.24 min, Rc： 36.18 min, Rb2：38.55 min and Rd： 40.88 min） with those of the standards under the same chromatographic conditions, which showed similar results among the samples of six different batches and among the samples from one batch detected six times within one day. Conclusions： Xinyue Capsules have good drug intra-day consistency at room temperature and exhibit a consistent quality between different batches. This study established a reliable method to assess the stability of Xinyue Capsules, which is suitable for further qualitative analysis and may assist in promoting the safe and effective use of Chinese herbal medicine.

Absorption of Curcumin Monophosphate in Rat Intestinal Circulation

[Objectives] This study aimed to study the absorption of curcumin monophosphate, a derivative of curcumin, in the small intestine of rats. [Methods] In situ recirculation perfusion technique was used to study the absorption of curcumin monophosphate in intestinal circulation of rats, and the content of curcumin monophosphate in intestinal circulation solution was determined by high-performance liquid chromatography/ultraviolet detector(HPLC/UV). [Results] The established HPLC/UV method has good specificity. Linear regression was conducted between the peak area of curcumin monophosphate(A) and the concentration of curcumin monophosphate(C). The established standard curve equation was y=30.07x+102.48(R^2=0.999 0), indicating that curcumin monophosphate has good linearity in the range of 1.25-100.00 μg/mL. After excluding the degradation of the drug and the loss of sampling, within the first 2 h of the experiment, the drug absorption in the small intestine of rat was 1.39 mg, accounting for 97.2% of the total drug absorption during the 5-h experimental period, and the absorption rate was 53.9%.[Conclusions] Curcumin monophosphate has a good absorption in the small intestine of rats.

超声提取-高效液相色谱法测定化妆品中5种苯并三唑类紫外线吸收剂

建立了一种利用高效液相色谱同时测定化妆品中甲酚曲唑(UV-P)、奥克三唑(UV-329)、布美三唑(UV-326)、甲酚曲唑三硅氧烷(DTTSO)、亚甲基双-苯并三唑基四甲基丁基酚(UV-360)的方法。其中,水状化妆品经甲醇/四氢呋喃溶解、超声提取、微孔滤膜过滤后进样;乳液状、霜状化妆品经甲醇/四氢呋喃溶解、涡旋振荡、超声提取、微孔滤膜过滤后进样。使用ZORBAX SC-C18色谱柱(250 mm×4.6 mm,5μm),柱温23℃,以0.1%的甲酸水溶液为A相、甲醇为B相、四氢呋喃为C相进行洗脱,流速1.0 mL/min,检测波长340 nm,进样量5μL。结果表明,5种紫外线吸收剂在11~176 mg/L的质量浓度范围内线性关系良好(R2≧0.9994),检测限分别为6.72,11.94,13.80,18.47和23.49μg/L,相对标准偏差小于1.7%(n=6),加标平均回收率达到93.7%~104.5%。该方法能满足化妆品中5种苯并三唑类紫外线吸收剂的测定。

高效液相色谱法测定皮革中7种苯并三唑类防紫外线稳定剂

建立了高效液相色谱法测定皮革产品中7种苯并三唑类防紫外线稳定剂迁移量的方法。该方法采以甲醇作为提取溶剂,通过超声萃取,采用外标法进行定量,试验结果表明:7种目标物能够被有效分离,目标物浓度在0.1~30.0 mg/L范围内与峰面积呈良好的线性关系,线性相关系数均在0.99907以上,检出限在0.33~0.99 mg/kg。方法的平均回收率为85.98%~94.13%,相对标准偏差为2.58%~4.05%。该方法准确可靠,适用于皮革产品中苯并三唑类防紫外线稳定剂的检测分析。

高效液相色谱法同时测定僵蚕中4种核苷类成分

建立高效液相色谱法测定僵蚕中尿苷、次黄嘌呤、腺嘌呤和腺苷的分析方法。样品用水提取后,用Polaris 5 C8-A色谱柱(250 mm×4.6 mm,5μm)分离,以甲醇-水为流动相梯度洗脱,流量为1.0 mL/min,柱温为30℃,采用紫外检测器检测,检测波长为260 nm,以色谱峰面积外标法定量。尿苷、次黄嘌呤、腺嘌呤和腺苷质量分别在0.041~0.305μg、0.047~0.350μg、0.040~0.298μg、0.041~0.310μg范围内与色谱峰面积线性关系良好,相关系数均大于0.9996,测定结果的相对标准偏差为1.2%~2.1%(n=6),样品加标平均回收率为94.6%~97.9%。该方法有助于僵蚕药材及其饮片的质量标准提高。

In-situ carbonizing of coal pitch on the surface of silica sphere as quasi-graphitized carbon stationary phase for liquid chromatography

A novel chromatography stationary phase with a quasi-graphitized carbon modified shell has been developed. Coal pitch was directly carbonized on the surface of porous silica with in-situ carbonization. The carbonized coal pitch coating exhibits some degree of graphitization with a 78 nm-thick layer on the surface of silica and a 0.5 nm-thick layer on the inner surface of the mesopores. Based on the special structure of the graphitized carbon coating, the novel stationary phase can provide multiple interactions such as hydrophobic interaction, π-π interaction and dipole-dipole interaction. The novel composite material exhibited unique separation selectivity and excellent separation efficiency for polar compounds, including imidazoles, nucleosides and pesticides. Besides, the packed column also exhibited great repeatability with the RSDs of the retention time of nucleosides between 0.07%-0.50%(n = 5). Finally, satisfied result was achieved in the separation of fullerenes on the new column, suggesting the great potential in the industrial-scale purification of fullerenes.