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1.
??Chrysanthemum morifolium has a long history of culture and use in China. Due to different germplasm resources, producing areas, and processing methods, many cultivated varieties have formed now. The varieties and processing methods of C. morifolium are affected by economic interests and processing cost, which change gradually. On the basis of spot investigation and related literature study, the changes of the varieties and processing methods of C. morifolium were summarized in this paper. It will provide theoretical evidence for the culture, processing, quality evaluation, and clinical application of C. morifolium.  相似文献   

2.
??OBJECTIVE To study the monthly dynamics of physical and chemical indexes in Achyranthis Bidentatae Radix(ABR, the dried root of Achyranthes bidentata Bl.) stored in simple and cool warehouses. METHODS ABR was stored in simple and cool warehouses for 27 months. The color was observed. The water content was determined based on the drying method. The contents of ??-ecdysone and 5-hydroxymethylfurfural (5-HMF) were determined by HPLC method. The accumulation of temperature difference between the simple and cool warehouses was evaluated with a relative temperature cumulation (RTC) method. The monthly dynamics of physical and chemical indexes of ABR was analyzed with RTC. RESULTS As the extension of storage time, the ABR stored in the simple warehouse showed deeper color and harder texture, but the ABR stored in the cool warehouse still had soft texture without significant color change. The contents of ??-ecdysone in ABR stored in the two warehouses both gradually decreased and dropped to lower than the limit of 0.030% ruled by China Pharmacopoeia when being stored for up to 27 months. The contents of 5-HMF of ABR stored in the two warehouses both increased and were higher for the sample in the simple warehouse than that in the cool warehouse. CONCLUSION The concept of RTC is put forward and used to study the monthly dynamics of chemical constituents in traditional Chinese medicine during storage for the first time. The physical and chemical indexes of ABR varies during storage. Two years of storage time of ABR is suggested.  相似文献   

3.
??OBJECTIVE To discuss the problem of instrumental test method of clarity and degree of opalescence of liquids in the general notice 0902 of China Pharmacopeia(Ch.P)2015, find out the causes and offer solutions. METHODS The test methods of clarity in Ch.P 2015 and European Pharmacopeia (EP) 8.0 were compared, including instrumental types, applicability, sample requirements, and result evaluation. RESULTS The primary opalescent suspension for the instrumental method is the same as the visual method, using the absorbance (A=0.12-0.15) at 550 nm to control the opalescence. Because the resolving power of the instrumental method is far higher than the visual method, the limit becomes interval distribution instead of simple point. The opalescent value (NTU) of the upper limit (A=0.15) is about 1.35 times of the lower limit (A=0.12).When the NTU value of the test liquid is in this interval, the result evaluation will be hard.CONCLUSION The preparation of the primary opalescent suspension in Ch.P 2015 is different from EP8.0. For this reason, the limit set by Ch.P 2015 is actually stricter than that of EP8.0. The opalescent value of the standard solution used by Ch.P 2015 is about 75% of that used by EP8.0.  相似文献   

4.
??OBJECTIVE To determine the optimum ultrasonic-assisted extracting process of total flavonoids from Zingiber mioga by response surface methodology, and then study the antioxidant activity of the extract. METHODS On the basis of single factor experiments, a 4-factor, 3-level Box-Behnken center-united experiment was conducted. The Box-Behnken experiment analyzed and optimized the processing conditions by response surface methodology, then the antioxidant activity of the extract was determined. RESULTS The optimum conditions at ultrasonic power of 300 W were as follows treatment temperature 60 ??, ethanol concentration 85.99%, liquid-to-solid ratio 98.08 mL??g-1, treatment time 15 min. Under the optimum conditions, the extraction rate of the total flavonoids was 37.01%, with a bias of 4.28% compared with the predicted value of 35.49%; the reducing power of the total flavonoids from Zingiber mioga at the concentration of 1.038 7 mg??mL-1 was equal to that of vitamin C of 56.60 ??g??mL-1; the ??OH radical scavenging ratio of the total flavonoids from Zingiber mioga was 73.07%, the DPPH radical scavenging ratio was 65.72%, and the inhibition rate of anti-lipid peroxidation was 49.94%. CONCLUSION The total flavonoids from Zingiber mioga can be developed as a new type of antioxidant agents, and regression analysis and parameter optimization of the extracting process can be conducted by using response surface methodology.  相似文献   

5.
??OBJECTIVE To develop an LC-MS/MS method for the determination of vonoprazan pyroglutamate and vonoprazan fumarate in rat urine to determince the urine excretion of the two drugs in SD rats. METHODS The detection was performed on an API 4000 tandem mass spectrometer equipped with an electrospray ionization (ESI) source. Multiple reaction monitoring (MRM) was selected with the transitions of m/z 346.2 to 315.2 for TAK-438 P and m/z 237.2 to 194 for IS, respectively. Separation of the analytes was achieved by a Shimadzu liquid chromatography system with an Agelient C18 analytical column (4.6 mm??150 mm, 3.5 ??m). Isocratic elution was adopted with mobile phase A (10 mmol??L-1 ammonium acetate and 0.1% formic acid) and mobile phase B (methanol) at the ratio of 40??60, at a flow rate of 0.6 mL??min-1. The total run time was 6 min and the injected sample volume was 5 ??L. All the features of the developed method suggested it met the criteria for bioanalytical METHODS recommended by regulatory authorities. The accumulative urine excretion rates of TAK-438 F and TAK-438 P were determined after oral administration of TAK-438 P and equimolar TAK-438 F in SD rats.RESULTS The accumulative urine excretion rates of the prototype drugs were 2.11% and 2.03%, respectively. The low excretion rates indicated that metabolism might be the major clearance mechanism of TAK-438 P and TAK-438 F. CONCLUSION This was the first time to establish and validate a simple, rapid and sensitive LC-MS/MS method for the quantification of TAK-438 P. There is no significant difference of the accumulative urine excretion rate between TAK-438 P and TAK-438 F in SD rats, which provides the basis for the druggability of TAK-438 P.  相似文献   

6.
??OBJECTIVE To design and synthesize a series of oleanolic acid analogs posessing anti-tumor activity based on survivin target. METHODS Using the techniques of computer-aided drug design, the docking of Survivin and known active small molecules was simulated and then the key amino acid residue fragment of the target protein was analyzed. It led to the discovery of active groups capable of binding to the critical sites. Through using the natural product, oleanolic acid, as a lead compound, the active groups were introduced onto its A-ring, and the carboxyl group at the C-28 position was modified using amidation. SGC-7901 and A549 cells were used to screen the antitumor activity in vitro through the standard MTT method. RESULTS Ten new oleanolic acid derivatives were designed and synthesized,and their structures were confirmed by MS and NMR. The compounds ??5 and ??5 exhibited more potent cytotoxicity than the positive control drugs. CONCLUSION The novel oleanolic acid analogues have better antitumor activity than the parent compound, which are worthy of further study.  相似文献   

7.
??OBJECTIVE To design and synthesize brain targeting danshensu (DSS) derivatives and study their metabolism in rat plasma and brain homogenate in vitro. METHODS Tetramethylpyrazine and its derivatives were selected as carriers to design the brain targeting danshen suderivatives. Lipid-water partition coefficient (logP), brain blood concentration ratio (BB), and P-glycoprotein affinity of the derivatives were predicted by some calculation softwares and the better compound DT3 was chosen for the next synthesis. The degradation of DT3 and its intermediate DT1 in rat plasma and brain homogenate were measured by HPLC-UV. RESULTS Two danshensu-pyrazine ester derivatives were synthesized, ie DT1 and DT3. A simultaneous determination method of DT3, DT1, and (3,5,6-trimethylpyrazine-2-yl)methanol (TMPM) in rat plasma and brain homogenate was established. The degradation of DT3 in rat plasma and brain homogenate underwent the following processDT3??DT1??the active metabolites of DSS and TMPM.Compared with DT1, the degradation of DT3 in rat plasma slowed down.The half-lives (t1/2) of TMPM were 1.68 and 1.71 min, respectively. Also,DT3 could quickly release the active metabolitein rat brain homogenate, and the concentration of TMPM showed a steady increase with a t1/2 of 222.88 min. CONCLUSION The danshensu-pyrazine ester derivative DT3 has an extended t1/2 in rat plasma, and it can be degraded to active metabolite quickly in rat brain homogenate.  相似文献   

8.
??OBJECTIVE To evaluate the bioequivalence of cefdinir suspension and reference cefdinir capsule in Chinese healthy male subjects.METHODS A single oral dose of 100 mg cefdinir suspension or cefdinir capsule was given to 24 subjects according to a 2-way crossover design. The plasma concentrations of cefdinir were determined by UPLC-MS/MS. The pharmacokinetic parameters were calculated and bioequivalence was compared by WinNonlin 6.3 program. RESULTS The main pharmacokinetic parameters of cefdinir suspension and cefdinir capsule were as follow: ??max were (1 034.78??358.17), (969.71??297.38) ng??mL-1;tmax were (2.98??0.60), (3.44??0.70) h; AUC0-12 were (4 911.24??1 675.30), (4 522.35??1 600.13) ng??h??mL-1; AUC0-?? were (5 026.24??1 735.32),(4 680.69??1 699.93) ng??h??mL-1;t1/2 were (1.71??0.23), (1.79??0.39) h. The 90% confidential interval of ??max, AUC0-12, AUC0-?? of tested formulation were 95.6%-115.3%, 99.9%-117.2%, 99.0%-116.0%. CONCLUSION The two formulations are bioequivalent.  相似文献   

9.
??OBJECTIVE To prepare ion-sensitive ophthalmic in situ gel containing bendazac lysine (BDZL-ISG) and preliminarily study its rheological behavior, in vitro drug release, corneal permeation, and pharmacokinetics in rabbit aqueous humor. METHODS Single factor investigation was carried out to optimize the formulation, taking viscosity and gelling capacity as evaluation indices. Using aqueous solution or eye drops as control, the in vitro release of the formulation was evaluated by dialysis membrane method. Then, the corneal permeation experiment of the optimum formulation was carried out with Franz diffusion cell. The pharmacokinetics of BDZL-ISG in rabbit aqueous humor was preliminarily studied by microdialysis. RESULTS Compared with the control group, the optimum formulation had shear thinning behavior and significant sustained release effect. There was no significant difference in the corneal permeation between the two groups. The RESULTS of pharmacokinetic study showed that ??max (13.25 ??g??L-1) and AUC0-t of BZDL-ISG were 2.38 and 2.2 times higher than those of BDZL eye drops respectively, which suggested that the ocular bioavailability of BDZL was greatly enhanced by the optimum in situ gel formulation. CONCLUSION With significant sustained release effect, the ion-sensitive ophthalmic in situ gel will become a promising alterative formulation for bendazac lysine for treatment of cataracts.  相似文献   

10.
??OBJECTIVE To establish the HPLC fingerprints of Feijiehe pills and provide a foundation for its quality control and evaluation. METHODS A gradient elution method was applied. Ten batches of samples were analyzed by HPLC on a Diamonsil C18 (4.6 mm??250 mm,5 ??m) column with mobile phase composed of acetonitrile-0.01% phosphoric acid solution at a flow rate of 0.8 mL??min-1, the detection was carried out at 270 nm, and the column temperature was maintained at 25 ??. RESULTS There were 10 common peaks in the HPLC fingerprints. The similarity between peaks was more than 0.90. CONCLUSION The method is simple, accurate, reliable, and suitable to be applied to the quality control of Feijiehe pills.  相似文献   

11.
??OBJECTIVE To establish a determination method of molecular-size distribution of human serum albumin (HSA) by ultra performance liquid chromatography (UPLC).METHODS An UPLC method was developed to specifically determine the polymers and other components in HSA on UPLC PROTEIN BEH SEC analysis column with Waters Alliance UPLC system and Waters UPLC TUV detector. The separation was performed using a mobile phase consisting of PBS at a flow rate of 0.6 mL??min-1 and the UV detection wavelength was set at 280 nm. HSA samples were diluted to different concentrations (0.5-20 mg??mL-1) to confirm the optimal concentration range of the injection. The change of component percentage and the linear relationship between HSA concentration and chromatographic peak height were confirmed and the molecular-size distribution was calculated by area normalization method. Within the optimum injection concentration range, the national control sample for HSA was diluted to 12 mg??mL-1 and tested by UPLC method and the methodology was confirmed. Twenty batches of HSA samples were determined by both UPLC and existing HPLC methods, and the samples were determined in parallel. The consistency of the methods was compared and the method was reconfirmed.RESULTS The UPLC retention time of HSA polymer was 1.469 min, of dimer was 1.972 min, and of monomer was 2.267 min, respectively. The resolution of dimer and monomer was 2.20 and the USP tailing of monomer peak was 1.18 respectively. In the range of the injection concentrations, 0.5-20 mg??mL-1, there was linear relationship between the concentrations of the components of 11 HAS samples, including polymer, dimer and monomer peak, and the peak area%, peak height, peak area, and the squares of linear correlation coefficient were all greater than 0.997 0. The components peak area percentage of HSA samples remained relatively stable within the concentration range of 10-16 mg??mL-1 (total injection amount of 100-160 ??g). The RSDs of the percentage of polymers were 0.00% (n=3, 10 mg??mL-1), 0.10% (n=3, 12 mg??mL-1), and 0.10% (n=3, 16 mg??mL-1), respectively. The UPLC method was used to determine the national control sample for human albumin of 12 mg??mL-1, and the mean value of peak area% was 5.62% (n=10). The results were consistent with those of the parallel determination by HPLC (5.58%), both of which were in accordance with the quality control range of the national standard for human albumin. The RSD of the percentage of the peak area of the polymers in national standard for human albumin by UPLC was 0.40% (n=10). The HPLC and UPLC methods were used to determine the polymer peak area percentage of 20 batches of HSA samples from 7 domestic and foreign enterprises at the concentration of 12 mg??mL-1. The correlation coefficient of the two methods was 0.996 0 (P> 0.05) and there was no significant difference between the two methods (P>0.05).CONCLUSION Compared with the traditional HPLC method, the detection time of HSA SEC by the proposed UPLC method is shortened by at least 10 times, and the accuracy and repeatability of the determination are satisfactory. UPLC method can save much more analysis time, is simple and much faster, and can be used for high-throughput determination of molecular-size distribution of human serum albumin.  相似文献   

12.
目的采用超高效液相色谱与串联四级杆飞行时间质谱仪联用技术(U PLC/Q-TOF MS/MS)对蛇床子超临界提取物的体内外成分进行分析和鉴定。方法用ACQUITY UPLC BEHC18色谱柱,以0.1%甲酸水溶液(A)-乙腈(B)为流动相梯度洗脱,检测波长254 nm,使用ESI离子源,在正离子模式下采集数据;采用与标准品对比和质谱数据分析及检索文献的方法鉴定化学成分。结果检测出蛇床子超临界提取物中9个化合物,其中5个成分经过鉴定确认均为香豆素类,大鼠口服蛇床子提取物的血浆中检测出欧前胡素和蛇床子素两个原形成分。结论 UPLC/Q-TOF MS技术快速有效,具有较高的灵敏度和分辨率,适宜于鉴定中药复杂的体内外活性成分。  相似文献   

13.
??OBJECTIVE To establish the fingerprint of Aconitum Flarum Hand. Mazz Busch. METHODS UPLC analysis was performed on ACQUITY UPLC BEH C18 column(2.1 mm??50 mm,1.7 ??m). Gradient elution was conducted. Mobile A was 0.2% formic acid and 0.005% TFA in water; mobile B was methanol; and mobile C was acetonitrile. The flow rate was 0.3 mL??min-1. The detection was carried out at 275 nm. The column temperature was maitained at 35 ??. The injection volume was 1.0 ??L. RESULTS The UPLC fingerprint of Aconitum Flarum Hand. Mazz was established, and 14 common peaks were found including the peaks of two major constituents. The similarity factors ranged from 0.850 to 0.980. In addition, there was significant difference between wild and cultivated samples. CONCLUSION This UPLC method has satisfactory precision, stability, repeatability and specificity. It provides a scientific method for identifying wild and cultivated Aconitum Flarum Hand. Mazz using fingerprint.  相似文献   

14.
??OBJECTIVE To establish an isobutyryl derivatization combined with UPLC-MS/MS method for the quantitative analysis of 5-aminosalicylic acid (5-ASA) in human urine.METHODS Urine sample was analyzed by UPLC-MS/MS after pretreatment with isobutyryl derivatization and precipitation with acetonitrile. The separation was performed on the ACQUITY UPLC?j BEH-C18 column (2.1 mm??100 mm,1.7 ??m) at 40 ?? with injection volume of 3 ??L. The mobile phase was acetonitrile-5 mmol??L-1 ammonium formate containing 0.075% formic acid (20??80) at a flow rate of 0.4 mL??min-1. Electrospray ionization (ESI) source was applied and operated in multiple reaction monitoring (MRM) mode with negative ionization using the transitions of m/z 222.0??178.1 and m/z 206.1??162.0 for isobutyl 5-ASA and isobutyl 3-amino benzoic acid (3-ABA, IS), respectively.RESULTS The method was specific and sensitive. It exhibited good linearity over the concentration of 0.100-30.0 ??g??mL-1 for 5-ASA with the LLOQ of 0.100 ??g??mL-1, extraction recovery of 101.7%-115.4% and normalized matrix factor of 1.000-1.025. The intra- and inter-day precisions were both less than 15%.CONCLUSION The method is specific, simple, accurate and stable for quantitative analysis of 5-ASA in human urine.  相似文献   

15.
??OBJECTIVE To establish the UPLC fingerprint of Gardeniae Fructus for providing reference for effective quality control. METHODS The samples were analyzed on a Waters ACQUITY UPLC BEH C18 (2.1 mm??50 mm,1.7 ??m) column maintained at 30 ?? and eluted with methanol and water containing 0.02% phosphoric acid as mobile phases in a linear gradient mode.The flow rate was set at 0.4 mL??min-1 and the injection volume was 0.2 ??L. The detection wavelengths were set at 238 nm (0-5.4 min) and 440 nm (5.4-10 min).RESULTS The fingerprints of 16 batches of samples were analyzed with similarity evaluation, principal component analysis (PCA) and partial least squares discriminant analysis (PLS-DA). The common mode of the fingerprint was established with 24 common peaks, and four of them were identified, which were genipin 1-gentiobioside (4), gardenoside (6), crocin ?? (15), and crocin ?? (17). The similarity degrees of the 16 batches of samples were between 0.986 0 and 0.995 0. The samples were divided into two groups, ZheJiang (S1-S6) and other areas (S7-S16), analyzed by principal component analysis (PCA) and partial least squares discriminant analysis (PLS-DA). Eleven significantly different components were found, including genipin1-gentiobioside, gardenoside, crocin ??, crocin ?? and some others. CONCLUSION The establishment of UPLC fingerprint of Gardeniae Fructus from different producing areas and the application of chemical pattern recognition can provide more comprehensive references for the quality control and evaluation of genuine Gardeniae Fructus from Zhejiang Province.  相似文献   

16.
??OBJECTIVE To develop and verify a magnetic beads-based extraction combined with quantitative PCR(q-PCR)method for determination of residual host cell DNA in recombinant human albumin products expressed in Pichia pastoris. METHODS The residual Pichia pastoris host cell DNA in samples were extracted by magnetic beads-based extraction method and then determined by Taqman probe-based q-PCR. The residual DNA content was calculated according to the standard curve. The developed method was verified for accuracy and precision with different derivation albumin matrixes and concentrations, and the residual DNA of 3 batches of recombinant human albumin products expressed in Pichia pastoris were detected. RESULTS The minimum detection limit of Pichia pastoris residual DNA by the developed method was 3 fg??L-1, the linear range was 3 fg??L-1-300 pg??L-1, and the correlation coefficient(r2) was 0.998 3. The recovery rates of spiked samples in rHA matrix were 93.58%(RSD 19.6%, n=4)at 100 fg??L-1 and 215.56%(RSD 42.9%, n=4) at 10 fg??L-1, respectively. The recovery rates of spiked samples in HSA matrix were 67.09%(RSD 6.9%,n=3)at 100 fg??L-1 and 113.40%(RSD 11.1%, n=3) at 10 fg??L-1, respectively. The residual Pichia pastoris DNA contents in 3 batches of recombinant human albumin products expressed in Pichia pastoris determined by the developed method were 5.98, 4.16, 4.49 fg??L-1(n=7) respectively and not more than 1 ng per 10 g protein. CONCLUSION Magnetic beads extraction method combined with fluorescence quantitative PCR method solves the technical problem of quantitative determination of trace DNA in recombinant human albumin products with ultra-high concentration protein. The method is accurate and reproducible, and can be used for quantitative determination of DNA residue in recombinant human albumin expressed by Pichia pastoris.  相似文献   

17.
??OBJECTIVE To establish the UPLC fingerprint of Cistanche deserticola Y.C. Ma and Cistanche tubulosa (Schrenk) Wight.METHODS The UPLC fingerprints of 10 batches of C. deserticola and C. tubulosa were determined on an ACQUITY UPLC BEH C18 column (2.1 mm??50 mm,1.7 ??m) eluted with the mobile phase consisting of 0.2% formic acid solution and acetonitrile in gradient mode at a flow rate of 0.4 mL??min-1, the column temperature was 40 ??, and the detection wavelength was set at 240 nm. The chemical attribution of the fingerprint was determined by reference substance comparison method. RESULTS The common mode of the UPLC fingerprint of C. deserticola and C. tubulosa was set up under the established conditiom. There were 15 common peaks in the fingerprints of 10 samples, five of which were identified. The similarities varied from 0.667 to 0.905 and from 0.249 to 0.991 for Cistanche deserticola Y.C. Ma and Cistanche tubulosa (Schrenk) Wight, respectively. There was significant difference in the fingerprints between C. deserticola and C. tubulosa. CONCLUSION The method is simple and reliable, which can be readily utilized for distinguishing C. deserticola from C. tubulosa and their quality control.  相似文献   

18.
??OBJECTIVE To prepare the first batch of Chinese national standard for human albumin used for the test of batch release or other quality control of human albumin products.METHODS The first batch of national standard for human albumin was prepared with certificated human albumin products, mixed and filled under aseptic conditions. The standards were distributed to 11 laboratories for cooperative calibration according to the unified methods published on China Pharmacopeia.Seven test items including total protein content, sodium caprylate, polymers content, pH,absorbance,sodium content, and aluminium content were detected. RESULTS The limits of the six test items except aluminium content were established as follows after the data from 11 collaboration laboratories were received and statistically analyzed: total protein(193.30??5.08)g??L-1;sodium caprylate (0.162 4??0.009 2) mmol??g(Pro)-1; polymers content (2.72??0.29)%( HPLC-SEC);pH(6.71??0.08)[temperature (22??3)??];absorbance 0.030??0.005;sodium content (134.9??23.6)mmol ??L-1.The range of initially established aluminium content was (88.4??30.5)??g??L-1. However,it was observed to increase obviously after 21 months according to the trend analysis, so it was deleted from the test items for the national standard for human albumin ultimately.CONCLUSION The prepared national standard for human albumin met the relevant requirements and may be served as the first generation of national standard for human albumin products.  相似文献   

19.
??OBJECTIVE To investigate a rapid approach for quality evaluation of Huoxiang Zhengqi Tincture. METHODS Hesperidin, glycyrrhizic acid, imperatorin, honokiol, isoimperatorin, magnolol and atractylodin in Huoxiang Zhengqi Tincture were determined by ultra performance liquid chromatography (UPLC) method combined with wavelength switching detection technology. The sample was injected directly without preprocessing. The separation was performed on an ACQUITY UPLC BEH C18 (2.1 mm??100 mm, 1.8 ??m) and the column temperature was maitained at 40 ??. The mobile phase was composed of acetonitrile and 0.1% phosphoric acid with gradient elution at a flaw rate of 0.3 mL??min-1. Hesperidin was detected at 284 nm; glycyrrhizic acid was detected at 250 nm; imperatorin, honokiol, isoimperatorin and magnolol were detected at 300 nm; atractylodin was detected at 340 nm. RESULTS The calibration curves of the seven components showed good linearity within their test ranges. The average recoveries for hesperidin, glycyrrhizic acid, imperatorin, honokiol, isoimperatorin, magnolol and atractylodin were 99.3%, 99.5%, 101.5%, 99.3%, 100.6%, 99.0% and 99.6%, respectively. And there were great variations among the contents of glycyrrhizic acid, imperatorin, isoimperatorin and atractylodin in 28 batches of samples from 13 manufactures. CONCLUSION The proposed method is accurate, simple and rapid, thus providing basis for comprehensive quality control of Huoxiang Zhengqi Tincture.  相似文献   

20.
??OBJECTIVE To establish a method for rapid screening and quantification of 24 anti-inflammatory painkillers illegally added in traditional Chinese medicines and health foods by UPLC-quadrupole/electrostaticfield orbitrap high resolution mass spectrometry. METHODS The separation was performed on a Thermo Acquity UPLC system with a Hypersil Gold C18 column with gradient elution of acetonitrile and 20 mmol??L-1 ammonium acetate solution.Electrospray ionization of positive and negative ions and one and two high precision full scan were used for the MS detection. The qualitative and quantitative analyses were carried out by accurate and precise parent ion mass and product ion mass information. RESULTS The limits of detection(S/N??3) were 10.0-45.0 ??g??kg-1. The average recoveries were 79.6%-98.3%. Thirty positive samples were detected among a total of 45 samples, resulting a positive rate of 66.7%. The detected components were paracetamol, diclofenac sodium, indometacin, and ibuprofen. CONCLUSION The method is simple, highly accurate, sensitive and selective, and can be used in rapid screening and quantitative analysis of illegally added anti-inflammatory painkillers in traditional Chinese medicines and health foods.  相似文献   

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