91 results about "Hplc dad" patented technology

The invention provides a detection method for a fingerprint chromatogram of flavonoid and organic acid components in a ginkgo biloba extract. The detection method comprises the following steps: (1) preparing a test solution; (2) preparing a reference solution; (3) respectively determining the test solution and the reference solution by adopting high-performance liquid chromatography, and comparing the acquired fingerprint chromatogram with a standard fingerprint chromatogram to obtain the fingerprint chromatogram of the flavonoid and organic acid components in the test solution. The invention further provides the application of the detection method in the quality detection and the component test determination of the flavonoid and organic acid components in the ginkgo biloba extract. According to the detection method for the fingerprint chromatogram of flavonoid and organic acid components in the ginkgo biloba extract and the application of the detection method provided by the invention, the fingerprint chromatogram of flavonoid and organic acid medicinal components in the ginkgo biloba extract is established; the quality control level of the flavonoid and organic acid medicinal components in the ginkgo biloba extract is improved; effective quantitative analysis can be performed.

The invention discloses a method for simultaneously determining twenty-two flavones and phenolic acids in citrus fruits by adopting high performance liquid chromatography-diode array detector-fluorescence detector (HPLC-DAD-FLD). The method is capable of simultaneously determining twenty-two phenolic compounds in citrus fruits such as gallic acid, synephrine, chlorogenic acid, protocatechuic acid,caffeic acid, p-coumaric acid, rhamnosylvitexin, eriocitrin, ferulic acid, rutin, benzoic acid, narirutin, naringin, hesperidin, diosmin, neohesperidin, quercetin, naringenin, kaempferol, nobiletin,hesperetin, acacetin and the like, derivatization is not needed, and the method is high in accuracy, high in sensitivity and excellent in repeatability.

The related detection method for amino acid content in Xiasangju preparation comprises: (a) preparing reference solution; (b) preparing sample solution; (c) chromatogram condition: using octadecylsilicane chemically bonded silica as filler, using the gradient elution liquid with 0.05~0.10mol/L NaAc solution buffer and 20-80% acetonitrile solution as mobile phase with pH value as 4.50-5.05, 30-50Deg temperature, activation wavelength 250nm, emission wavelength 395nm, flow rate as 0.5-1.5mL .min-1, and 30-80min; (d) obtaining the fingerprint spectrum with HPLC. This invention is simple and stable, and has well repeatability and precision.

The invention discloses a method for creating a multi-index quantitative fingerprint spectrum for food retention-removing and cough-relieving oral solution for children, which includes the following steps: high-performance liquid chromatography (HPLC)-diode array detector-electrospray ionization-quadrupole-time of flight mass spectrometry combination is adopted to detect chemical information characteristic peaks of a variety of common chemical substances in multiple batches of food retention-removing and cough-relieving oral solution for children, and according to the detected chromatographic peaks of a variety of the common chemical substances in the multiple batches of retention-removing and cough-relieving oral solution for children in combination with multi-index ingredient content determination, a fingerprint spectrum of the food retention-removing and cough-relieving oral solution for children is created. The method adopts the HPLC-DAD-ESI-Q-TOF/MS technique to analyze and identify chemical ingredients in the food retention-removing and cough-relieving oral solution for children, quality control indexes are chosen in reference to the principle of concerted application of Chinese herbal medicines and by referring to individual herb quality control indexes in one volume of 2015 edition of Chinese Pharmacopoeia and an identification result of each common peak, an HPLC multi-index quantitative fingerprint spectrum is created on the basis, and thereby a relatively comprehensive method and technical support are provided for the research on the evaluation of the overall quality of the food retention-removing and cough-relieving oral solution for children.

The invention discloses a method using a derivatization HPLC-DAD method to determine small-molecule halogenated carboxylic acid in medicine.The method includes: under normal temperature, using nitrobenzene hydrazine derivatization reagent to derivatize the small-molecule halogenated carboxylic acid so as to generate products with high absorption in the ultraviolet visible region; using the reaction liquid after the derivatization reaction as the feeding sample, and using the HPLC-DAD method to determine the derivatization products of halogenated carboxylic acid in the feeding sample in the ultraviolet visible region on the basis of the reversed phase partition chromatography principle so as to achieve the qualitative or quantitative detection of the small-molecule halogenated carboxylic acid.Due to the fact that the ultraviolet absorption band of the carboxylic acid derivatization products of the nitrobenzene hydrazine derivatization reagent has evident redshift effect due to the existence of nitro electron-withdrawing group on benzene ring and most medicine and impurities thereof are weak in absorption in the ultraviolet visible region (300-450 nanometers), the simple and universal method using pre-column derivatization HPLC-DAD to determine the small-molecule halogenated carboxylic acid is built.Methodology validation shows that the method is good in specificity.

The invention discloses a method for detecting acyl chloride in a medicine or synthesized intermediate thereof by a derivatization HPLC-DAD method. The method comprises the following steps: derivatizing acyl chloride with a nitrophenylhydrazine derivatized reagent at room temperature to generate a product has relatively absorbability in an ultraviolet visible region; separating and detecting the derivatized product of acyl chloride in the ultraviolet visible region by using the derivatized reacting liquid as a feeding sample based on the principle of reversed-phase high-performance liquid chromatography so as to qualitatively or quantitatively detecting acyl chloride. Based on the quick reaction characteristic of acyl chloride and hydrazino and the ultraviolet visible absorption characteristic of the product generated after acyl chloride and nitrophenylhydrazine perform a biochemical reaction, interference of a medicine or the synthesized intermediate matrix thereof on acyl chloride detection can be effectively avoided, so that a simple and universal method for detecting acyl chloride in a medicine or synthesized intermediate thereof by a derivatization HPLC-DAD method can be established. Methodological verification results indicate that the method has excellent specificity and sensitivity.

The invention discloses a magnetic solid-phase extraction method of detecting ethoxyquine in fruits and vegetables. The method uses a magnetic covalent organic skeleton material Fe3O4@COF(TpDA) as anadsorbent for magnetic solid-phase extraction, so as to extract ethoxyquine in fruits and vegetables. The method detects PGRs in fruits and vegetables by using an MSPE technology, and selects Fe3O4@COF(TpDA) as the adsorbent. The adsorbent is convenient to use, has multiple carbonyl and aromatic rings on the surface, can enrich and extract PGRs through hydrophobic interaction, pi-pi interaction and hydrogen bonds, has good extraction effect and high structure stability, can be reused, and can detect multiple trace PGRs in fruits and vegetables sensitively. In the method, MSPE of Fe3O4@COF(TpDA) and HPLC-DAD are combined for the first time for measuring PGRs, providing a new concept for detection of PGRs.

The invention relates to a quality control method of a mangnolia officinalis refined medicinal slice. The quality control method comprises the following steps that: the content of the mangnolia officinalis refined medicinal slice is determined by taking magnolol and a magnolol comparison product as comparisons through a high-performance liquid chromatography; the geoherbalism of contained mangnolia officinalis is determined by taking magnolol and magnolol as reference objects and taking relative retention time and relative retention peak area of a common peak of a high-performance liquid fingerprint through a high-performance liquid fingerprint method; the fact that whether the mangnolia officinalis exists and the content of the mangnolia officinalis can be detected; furthermore, the geoherbalism of the mangnolia officinalis is also further detected; and, due to specificity of traditional Chinese medicines, effects and performances of medicines are directly influenced by the geoherbalism of raw materials, which is recognized in the field; therefore, the quality control method disclosed by the invention is capable of ensuring that the quality of the mangnolia officinalis refined medicinal slice is steadier and more reliable.

The invention discloses a fingerprint spectrum detection method and a fingerprint spectrum of a Yixinshu preparation. The fingerprint spectrum detection method comprises the following steps: by taking a schizandrin reference substance as reference, measuring the fingerprint spectrum by adopting high performance liquid chromatography (HPLC). The similarity of the HPLC fingerprint spectrum of the Yixinshu preparation established in the method and a reference spectrum is more than 0.9, the quality of the fingerprint spectrum can be effectively characterized, and the product quality is comprehensively monitored. Moreover, a common mode of the HPLC characteristic fingerprint spectrum of the Yixinshu preparation is established, 15 common peaks are calibrated, the established fingerprint spectrum is high in technical content, the simplicity and one-sidedness of the quality control of the Yixinshu preparation are avoided, and the possibility that the quality of the artificially handled product reaches the standard is reduced.

The invention discloses a method for evaluating color, flavor and taste multicomponent quantification combination fingerprint quality of saffron. According to the method, first an HPLC-DAD-ESI-MSn technology is adopted to analyze and identify representative ingredients of color, flavor and taste in the saffron which are crocin, safranal and picrocrocin and the like, and 7 crocins, picrocrocin, aglycone (HTTC) of picrocrocin, safranal and 2 kaempferols are identified as flavonoids of aglycone. On the basis of color, flavor and taste multicomponent and mass spectrum identification in saffron, a wavelength switching HPLC-DAD technology is utilized to construct the method for multicomponent quality evaluation through the color, flavor and taste multicomponent quantification combination fingerprint, comprehensive quality analysis can be performed on saffron, and clinical application safety and effectiveness of saffron are improved.

The invention relates to a method for chiral separation of various side chain protected amino acids, and aims to solve the technical problems that a mobile phase system used in an HPLC (high performance liquid chromatography) chiral separation system is complex and chiral HPLC columns are instable. According to the technical scheme, the method is characterized by including the steps of a, dissolving four racemates in methanol and water solution, performing ultrasonic treatment, filtering, and taking filtrate for standby; b, allowing well balanced chiral HPLC columns to respectively absorb the filtrate which is sent to the HPLC system, allowing a chromatographic work station to acquire chiral separation chromatograms, and checking separation parameters to acquire amino acid separation effects. Mobile phase used by the method is a common reagent in HPLC. A HPLC instrument needs no other instruments, cost is saved, and the various side chain protected amino acids can be chirally separated fast.

The invention discloses a detection method of a fingerprint spectrum of an astragalus membranaceus and poria cocos kidney invigoration tablet and the fingerprint spectrum of the astragalus membranaceus and poria cocos kidney invigoration tablet. According to the method, a standard fingerprint spectrum of the astragalus membranaceus and poria cocos kidney invigoration tablet is established; high performance liquid chromatography and gradient elution are adopted; the number of theoretical plates is calculated according to a sinomenine peak and is not less than 100000. The similarity between thefingerprint spectrum of the astragalus membranaceus and poria cocos kidney invigoration tablet obtained by the method and a control fingerprint spectrum is greater than 0.9; the fingerprint spectrum can comprehensively and effectively characterize quality of the astragalus membranaceus and poria cocos kidney invigoration tablet; a quality evaluation system of the astragalus membranaceus and poriacocos kidney invigoration tablet is perfected; the obtained fingerprint spectrum of the astragalus membranaceus and poria cocos kidney invigoration tablet has many characteristic peaks and is high insimilarity; the quality of the astragalus membranaceus and poria cocos kidney invigoration tablet can be monitored accurately and reliably; the detected fingerprint spectrum is recognized by a traditional Chinese medicine chromatographic fingerprint spectrum similarity evaluation system provided by Chinese Pharmacopoeia Commission; the fingerprint spectrum of the astragalus membranaceus and poriacocos kidney invigoration tablet is evaluated according to an obtained similarity result; a conclusion is relatively objective and accurate; and the method has the advantages that the method is simpleand convenient, excellent in stability, high in precision, good in repeatability and the like.

This invention discloses one Disheping quality test method, which can control its product quality effectively and tests the relative subject, mapping abnormal part content by use of effective liquid phase spectrum, wherein, the relative subject and abnormal structure provides test sample liquid spectrum peak area less than comparison main peak area and the content measuring is no less than 98.5 percent and the weight metal test is not more than ten of million and the dry loss is no more than 0.5 percent and the burst resides no more than 0.3 percent.

The invention discloses a method for identifying litchi honey. The method comprises the following steps: firstly, constructing an HPLC-DAD (High Performance Liquid Chromatography-Diode Array Detection) fingerprint chromatogram of litchi honey, chaste honey and rape honey so as to determine characteristic markers of the litchi honey; then, separating and purifying the determined characteristic markers according to a preparative liquid chromatography so as to respectively obtain two kinds of characteristic markers with higher purity; and finally, analyzing the molecule information of the characteristic markers by using a quadrupole/time-of-flight mass spectrometer so as to finally determine that the molecular weight of the two kinds of characteristic markers is 264 and the molecular formulais C15H20O4, thereby conjecturing that the two kinds of characteristic markers are isomers. The method disclosed by the invention is reasonable in design, and the selected analytical instrument is high in sensitivity, high in analysis speed, high in separation efficiency and highstrong in feasibility and provides a basis for authenticity identification and quality control of the litchi honey.

The invention discloses a solid phase micro-extraction method of unsaturated compounds. A silver nanoparticle functionalized monolithic column prepared by an in-situ reduction method is used a solid-phase micro-extraction monolithic column; and in combination with an in-tube solid-phase micro-extraction-high performance liquid chromatography-diode array on-line combined detection system (In-tube SPME-HPLC-DAD), a solid-phase micro-extraction new method of the unsaturated compounds is established. According to the solid phase micro-extraction method of the unsaturated compounds provided by theinvention, a special acting force existing between silver nanoparticles loaded in a monolithic column material and an unsaturated carbon-carbon double bond carried by the unsaturated compounds is usedto achieve the enrichment of the unsaturated compounds on the silver nanoparticle functionalized monolithic column; and since the strength of the acting force between silver nanoparticles and an unsaturated compound cis-trans-isomer is different, the sequential elution of the unsaturated compound cis-trans isomer is further realized, and the requirements for efficient detection of trans fatty acids and the separation and analysis of is-trans-stilbene are satisfied.

The invention relates to the technical field of clinical blood concentration monitoring of psychotropic drugs, in particular to an HPLC-DAD method for determinating quetiapine drug concentration of human serum. The invention provides a method for determinating the quetiapine concentration of the serum after a quetiapine drug is taken. The method comprises the following steps: pretreating a human serum sample and performing high-performance liquid chromatography (HPLC-DAD) analysis. The invention establishes the HPLC-DAD method with strong specificity, high sensitivity and high reproducibility.By the method for determinating the quetiapine blood concentration, established for the first time, verification results in aspects of accuracy, precision, specificity, stability and the like meet analytical requirements of the 2015 edition of relevant guiding principles of the Pharmacopoeia of the People's Republic of China (9012) on a biological sample.

The invention provides a high-performance liquid chromatography (HPLC) method based method for detecting kappa-casein typing in milk. A provided HPLC method can be utilized to perform typing on two variants which are AE-kappa casein and B-kappa casein in milk, so that the B type kappa casein which can enhancing cheese output can be obtained.

The invention provides a method for simultaneously determining four components in a herba cynomorii-containing sample, in particular to a method for simultaneously determining gallic acid, protocatechuic acid, catechin and phlorizin in the herba cynomorii-containing sample by using a high performance liquid chromatography (HPLC). According to the method, a standard product solution and a sample solution are determined by using the HPLC, and multi-gradient elution is carried out by using acetonitrile and 0.05% of a glacial acetic acid solution as mobile phases, so that the four components can be determined. Compared with the chemical composition determination method in the prior art, the method provided by the invention is simple in operation process, good in repeatability and high in accuracy, avoids the consumption of time and cost, can be used as an effective method for quantitatively controlling the quality of herba cynomorii, and is also used for detecting herba cynomorii-related effective components in Chinese patent medicines.

The invention discloses a quality determination method for an HPLC-DAD fingerprint spectrum of a eutrema wasabi maxim medicinal material. The method includes the steps: respectively preparing a test sample solution and a control substance solution prepared from a 3-butylene isothiocyanate control substance, a 5-methylthiopentyl-isothiocyanate control substance and a 6-methylthiohexyl-isothiocyanate control substance, and injecting the two solutions into a high performance liquid chromatographic instrument, and determining by gradient elution via a high performance liquid chromatography method,to obtain the fingerprint spectrum of the eutrema wasabi maxim medicinal material. According to the method, the eutrema wasabi maxim medicinal material is determined by gradient elution via the highperformance liquid chromatography method; the fingerprint spectrum of the eutrema wasabi maxim medicinal material is constructed, characteristic substances contained in the eutrema wasabi maxim medicinal material are truly reflected, and isothiocyanate compounds in the eutrema wasabi maxim medicinal material are analyzed and determined; and at the same time, the method is used as a quality controlmethod of the eutrema wasabi maxim medicinal material, and has the characteristics of good separation effect and high sensitivity.