Serum metabolomics study on benign liver lesions and hepatic malignancies by central carbon pathway metabolites / 药学实践杂志

Objective To screen potential metabolites and significantly altered metabolic pathways of liver lesions by central carbon pathway metabolites. Methods 32 healthy volunteers (HC), 23 patients with biliary cysts (CYST), 19 patients with biliary stones (Stone), 45 patients with hepatocellular carcinoma (HCC), and 50 patients with hilarcholangiocarcinoma (HCCA) were recruited. Their serum samples were collected for UPLC-QQQ-MS analysis and further MPP statistical analysis. Pattern recognition was further used to discovery the differences in metabolome between groups, and to explore the significantly altered metabolic pathway and possible pathogenic mechanism of liver diseases. Results A total of 15, 7, 7, and 3 metabolites and a total of 8, 4, 4, and 1 metabolic pathway that were significantly different in serum between CYST, Stone, HCC, HCCA and healthy controls were identified and enriched through serum metabolomics analysis, respectively. Conclusion According to the above identified differential metabolites and enriched metabolic pathway results, it is shown that liver lesions mainly involved in the energy metabolism and amino acid metabolism & transport, in addition, inositol phosphate metabolism were significantly changed both in CYST, Stone, HCC and HCCA.

Exploring Mechanism of Renshen Guben Oral Liquids in Treating Renal Fibrosis Based on Metabolomics and Network Pharmacology / 中国实验方剂学杂志

ObjectiveTo investigate the mechanism of Renshen Guben oral liquids（RGOL） in treatment of mice with renal fibrosis based on metabolomics and network pharmacology. MethodC57BL/6 mice were randomly divided into control group， model group and RGOL group， 12 mice in each group. Except for the control group， mice in the other groups were induced into unilateral ureteral obstruction（UUO） model by UUO. After preparation of the model， an aqueous solution of 4.2 g·kg-1 extract powder was administered by gavage to RGOL group for 14 d， and an equal amount of distilled water was administered by gavage to the control and model groups. After the last administration on the 14th day， urine was collected and detected by ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry（UPLC-QQQ-MS/MS） with 0.1% formic acid aqueous solution as mobile phase A， and acetonitrile-isopropanol（70∶30） as mobile phase B for gradient elution（0-1 min， 5%B； 1-5 min， 5%-30%B； 5-9 min， 30%-50%B； 9-11 min， 50%-78%B； 11-13.5 min， 78%-95%B； 13.5-14 min， 95%-100%B； 14-16 min， 100%B； 16-16.1 min， 100%-5%B； 16.1-18 min， 5%B）， column temperature of 40 ℃， flow rate of 0.4 mL·min-1， electrospray ionization（ESI）， collection range of m/z 50-900. Through network pharmacology， the targets of components in RGOL and the targets of renal fibrosis were analyzed interactively， and the key components and key targets were screened by network topology analysis， and DAVID platform was used to predict the signaling pathways of RGOL for the treatment of renal fibrosis. ResultA total of 7 differential metabolites involving 8 metabolic pathways were identified in RGOL for the treatment of renal fibrosis. The network pharmacology revealed that 36 key components in RGOL were related to 7 differential metabolites， mainly ginsenosides， notoginsenosides and nucleotides. Based on the herbs-components-targets-pathways network， a total of 23 key targets related to the treatment of renal fibrosis by RGOL were highlighted， which together with the differential metabolites were involved in linoleic acid metabolism， arginine biosynthesis， tricarboxylic acid cycle（TCA）， arginine and proline metabolism and other pathways. ConclusionBased on metabolomics and network pharmacology， this study preliminarily identified 7 differential metabolites， 36 potential pharmacodynamic components and 23 key targets and 4 key pathways in RGOL for the treatment of renal fibrosis， providing an experimental basis for the clinical application and mechanism study of this preparation.

Isolation and Identification of Arisaema Cum Bile Fermentation Strain and Preliminary Investigation on Its Compound Strain Fermentation / 中国实验方剂学杂志

ObjectiveIn order to solve the problem that the quality and stability of Arisaema Cum Bile in the fermentation process with hybrid bacteria were not easy to control， the microorganism in the fermentation process of Arisaema Cum Bile was isolated and identified， the dominant strains were screened and the fermentation process of Arisaema Cum Bile with compound bacteria was investigated. MethodThe submerged culture during the fermentation process of Arisaema Cum Bile was taken out for strain separation and purification. Bacteria and fungi multiphase identification and detection methods and automatic microbial analysis system were used to analyze and compare DNA sequences and identify microorganisms. The isolated and identified strains were respectively inoculated and fermented. After screening the dominant strains， a preliminary exploration of compound strain fermentation were carried out. The contents of index components in Arisaema Cum Bile fermented by compound strain and traditional Arisaema Cum Bile were compared by ultra-performance liquid chromatography-triple quadrupole tandem mass spectrometry （UPLC-QqQ-MS/MS）. Mmobile phase was 0.1% formic acid acetonitrile solution （A）-0.1% formic acid aqueous solution （B） for gradient elution （0-2 min， 35%-45%A； 2-10 min， 45%-48%A； 10-12 min， 48%-100%A； 12-12.01 min， 100%-35%A； 12.01-15 min， 35%-65%A）， the flow rate was set at 0.35 mL·min-1. The mass spectrographic analysis employed electrospray ionization （ESI）， negative ion acquisition mode and multiple reaction monitoring （MRM） scanning mode were adopted to collect information， the collection range was m/z 50-1 000. ResultEight microorganisms were isolated and identified from the submerged culture of Arisaema Cum Bile. Among them， Enterococcus sp. （anaerobic） and E. casseliflavus were selected as the dominant strains in the fermentation process. Compared with the traditional fermentation method， the contents of chenodeoxycholic acid， hyodeoxycholic acid and hyocholic acid in free cholic acid increased by 1.76， 0.06， 0.19 mg·g-1， respectively. In bound cholic acid， glycochenodeoxycholic acid， taurochenodeoxycholic acid， glycohyodeoxycholic acid， taurohyodeoxycholic acid， glycohyocholic acid， taurine porcine cholic acid decreased by 0.63， 0.23， 0.26， 0.16， 0.03， 0.04 mg·g-1， respectively. ConclusionArisaema Cum Bile with compound strain fermentation （Enterococcus sp. and E. casseliflavus） can be fermented more completely， the fermentation cycle can be shortened， and the quality and stability of products can be improved.

Qualitative and quantitative analysis of alkaloids in Eurycoma longifolia by HPLC-Q-TOF-MS combined with UPLC-QQQ-MS/MS / 中国中药杂志

A sensitive and efficient method was established and validated for qualitative and quantitative analysis of total alkaloids from the extract of Eurycoma longifolia by high-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry(HPLC-Q-TOF-MS) combined with ultra-performance liquid chromatography coupled with triple quadrupole tandem mass spectrometry(UPLC-QQQ-MS/MS). The HPLC-Q-TOF-MS conditions are as follows: Welch Ultimate XB-C_(18) column(4.6 mm×250 mm, 5 μm) with acetonitrile(containing 0.1% formic acid)-0.1% formic acid in water as mobile phase for gradient elution. The UPLC-QQQ-MS/MS conditions are as below: Agilent Eclipse Plus C_(18) column(2.1 mm×50 mm, 1.8 μm) with acetonitrile(containing 0.1% formic acid) and 0.1% formic acid in water as mobile phase for gradient elution. MS data were collected by electrospray ionization in positive ion mode. According to the comparison with reference standards and the accurate masses of molecules, a total of 17 alkaloids in E. longifolia extract were identified by HPLC-Q-TOF-MS. The UPLC-QQQ-MS/MS quantitative analysis result of 3 alkaloids showed that the linear ranges of them were good(r≥0.999 7) and the overall recoveries ranged from 108.8%-110.2%, with RSDs of 2.9%-5.3%. The method is accurate, reliable, and efficient, which can comprehensively reflect the constituents and content of alkaloids in E. longifolia. The result can serve as a reference for further elucidating its therapeutic material basis and quality control.

Effect of Steaming Time and Pressure on Contents of Six Ginsenosides in Ginseng Radix et Rhizoma by UPLC-QqQ-MS/MS / 中国实验方剂学杂志

Objective::The processing method of red ginseng was determined by comparing the effects of different steaming time and pressure on the total content of six ginsenosides. Method::The contents of ginsenoside Rg1, Re, Rf, Rb1, Rc and Rb2 were determined by ultra high performance liquid chromatography-triple quadrupole tandem mass spectrometry (UPLC-QqQ-MS/MS). The Waters ACQUITY UPLC BEH C8 column (2.1 mm×100 mm, 1.7 μm) was used. The mobile phase was 0.1% formic acid aqueous solution (A) and 0.1% formic acid acetonitrile solution (B) for gradient elution (0-4 min, 81%-79%A; 4-6.3 min, 79%-75%A; 6.3-6.5 min, 75%-71%A; 6.5-9.5 min, 71%A; 9.5-16.5 min, 71%-68.5%A; 16.5-16.6 min, 68.5%-60%A; 16.6-19 min, 60%-100%A). The flow rate was set at 0.4 mL·min-1 and the column temperature was set at 35 ℃. The mass spectrographic analysis employed electrospray ionization (ESI) and negative ion collection mode with capillary ionization voltage of 2.5 kV, desolvation temperature of 350 ℃, desolvation gas flow of 700 L·h-1 and cone gas flow of 50 L·h-1. Multiple reaction monitoring (MRM) mode was used to collect information, the collection range was m/z 100-1 500, detection was performed by MRM mode at m/z 799.59-637.49 for ginsenoside Rg1, m/z 945.54-475.79 for ginsenoside Re, m/z 799.59-475.49 for ginsenoside Rf, m/z 1 107.59-783.97 for ginsenoside Rb1, m/z 1 077.58-783.96 for ginsenoside Rc, m/z 1 077.75-191.19 for ginsenoside Rb2. Result::When the steaming time was 3 hours, the total mass fraction of six ginsenosides in each sample group was 7.099 8-16.768 5 mg·g-1, and the total amount of the six ginsenosides in atmospheric steaming was 2.5-12.6 times of that in pressurized steaming, which was obviously better than that in pressurized steaming. Conclusion::Under the conditions of this experiment, the best processing method of red ginseng is atmospheric steaming for 3 hours with fresh ginseng.

Simultaneous Determination of Four Alkaloid Components in Xiangbin Decoction by UPLC-QqQ-MS/MS / 中国实验方剂学杂志

Objective: To establish a quantitative method for the simultaneous determination of arecaine,arecoline,norisoboldine and boldine in Xiangbin decoction by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-QqQ-MS/MS), and compare the variation of their contents between single and mixed decoctions. Method: The separation was carried on a Waters ACQUITY UPLC BEH Shield RP18(2.1 mm×150 mm,1.7 μm)column, with 0.1%formic acid solution-acetonitrile as mobile phase for gradient elution. The flow rate was 0.2 mL·min-1, and the column temperature was 30℃. The quantitative MRM transitions of the four components were m/z 142.10/44.11 for arecaine,m/z 156.20/44.07 for arecoline,m/z 314.29/265.12 for norisoboldine and m/z 328.13/265.10 for boldine. The determination was performed in multiple reaction monitoring (MRM) mode by mass spectrometry with electrospray ionization (ESI) source under positive mode. Result: The linear ranges of arecaine,arecoline,norisoboldine and boldine were 0.479 0-57.48,0.976 0-78.08,0.812 0-64.96, 0.091 2-18.24 μg·L-1,respectively. The average recoveries of the above compounds ranged from 93.73%to 104.34%, with RSD (n=6) of less than 5%. The contents of arecoline,arecoline,norbibeldine and boltinine in Xiangbin decoction were (90.07±1.26),(445.27±12.39),(742.35±38.39),(38.50±3.33) μg·g-1,which were significantly lower than the contents in Linderae Radix and Arecae Semen. Conclusion: The method is rapid,sensitive,accurate and reproducible,and suitable for the simultaneous determination of multiple components in Xiangbin decoction,so as to provide a basis for the quality control of Xiangbin decoction. The compatibility of Xiangbin decoction has a significant effect on the dissolution contents of arecaine,arecoline,norisoboldine and boldine.

An UPLC-MS/MS method for simultaneous determination of multiple constituents in Guizhi Fuling capsule with ultrafast positive/negative ionization switching / 中国天然药物

Guizhi Fuling capsule (GFC), a traditional Chinese medicine (TCM) with effects of promoting blood circulation and dissipating blood stasis, has been widely used in the clinic. Because of the complex matrix and various chemical structure types, quality control of GFC remains great challenge. In the present study, an ultra performance liquid chromatography hybrid triple-quadrupole mass spectrometry (UPLC-QQQ MS) method with ultrafast positive/negative ionization switching was developed for simultaneous determination of 18 bioactive components in GFC, including methyl gallate, ethyl gallate, oxypaeoniflorin, benzoic acid, albiflorin, paeonolide, paeoniflorin, 1, 2, 3, 4, 6-pentagalloylglucose, mudanpioside C, benzoyloxypaeoniflorin, benzoylpaeoniflorin, pachymic acid, amygdalin, cinnamaldehyde, paeonol, cinnamic acid, 4-hydroxybenzoic acid, and gallic acid. Separation was performed on an Agilent Zorbax Extend-C18 column (2.1 mm × 50 mm, 1.8 μm), using a gradient elution with acetonitrile and water containing 0.1% formic acid. Cholic acid was selected as the internal standard. This newly developed method was fully validated for linearity, precision, accuracy, and stability, and then applied to quality assessment of GFC. Finally, the batch-to-batch reproducibility of GFC samples was evaluated by the cosine ration and Euclidean distance method, which showed high quality consistency. The results demonstrated that the developed method pro vided a reasonable and powerful manner for quality control of GFC.

Simultaneous detemination of 8 terpenoids compounds in tripterygium wilfordii suspension cells by UPLC-MS/MS / 国际中医中药杂志

Objective To establish a UPLC-QQQ-MS/MS (ultra-high performance liquid chromatography triple quadrupole tandem mass Spectrometry) method for simultaneous detemination of 8 terpenoids compounds in Tripterygium wilfordii suspension cells. Methods The separation and analysis were performed on Water HSS T3 C18, with 0. 1％ acetic acid solution-acetonitrile as the mobile phase for gradient elution. The column temperature was set at 30 ℃ with flow rate was 0.3 ml/min. The electrospray ionization (ESI) source was applied and operated in alternating positive and negative mode. Multi-reaction monitor (MRM) mode was used to quantify the 8 compounds. Results The limits of detection and limits of quantitation in 8 compounds (triptolide, triptonide, dehydroabietlc acid, triptophenolide, demethylzeylasteral, tripteridine, pristimerin, celastrol) were 0.0096-0.2480 ng and 0.0192-0.4960 ng, respectively. The correlation coefficents (r) of calibration curves were 0.9966-0.9993. The average recovery rates were 95.04％-105.20％, and the relative standard deviation was 2.14％-6.31％. Conclusions The established quantitative method is simple, rapid, sensitive and accuracy. It can be used for simultaneous analysis of 8 terpenoids compounds in Tripterygium wilfordii suspension cells by using UPLC-QQQ-MS/MS, which affords methodology evidence for research and quality control of Triptervgium wilfordii Hook. f. and its plant tissue cultures.

An UPLC-MS/MS method for simultaneous determination of multiple constituents in Guizhi Fuling capsule with ultrafast positive/negative ionization switching / 中国天然药物

Guizhi Fuling capsule (GFC), a traditional Chinese medicine (TCM) with effects of promoting blood circulation and dissipating blood stasis, has been widely used in the clinic. Because of the complex matrix and various chemical structure types, quality control of GFC remains great challenge. In the present study, an ultra performance liquid chromatography hybrid triple-quadrupole mass spectrometry (UPLC-QQQ MS) method with ultrafast positive/negative ionization switching was developed for simultaneous determination of 18 bioactive components in GFC, including methyl gallate, ethyl gallate, oxypaeoniflorin, benzoic acid, albiflorin, paeonolide, paeoniflorin, 1, 2, 3, 4, 6-pentagalloylglucose, mudanpioside C, benzoyloxypaeoniflorin, benzoylpaeoniflorin, pachymic acid, amygdalin, cinnamaldehyde, paeonol, cinnamic acid, 4-hydroxybenzoic acid, and gallic acid. Separation was performed on an Agilent Zorbax Extend-C18 column (2.1 mm × 50 mm, 1.8 μm), using a gradient elution with acetonitrile and water containing 0.1% formic acid. Cholic acid was selected as the internal standard. This newly developed method was fully validated for linearity, precision, accuracy, and stability, and then applied to quality assessment of GFC. Finally, the batch-to-batch reproducibility of GFC samples was evaluated by the cosine ration and Euclidean distance method, which showed high quality consistency. The results demonstrated that the developed method pro vided a reasonable and powerful manner for quality control of GFC.

Simultaneous determination of thirteen constituents in Pientzehuang by UPLC-QQQ-MS / 中成药

AIM To establish a ultra-high performance liquid chromatography coupled with triple quadruple mass spectrometry (UPLC-QQQ-MS) method for the simultaneous content determination of notoginsenoside R1,ginsenoside Re,ginsenoside Rg1,ginsenoside Rb1,ginsenoside Rd,taurine,taurocholic acid,cholic acid,glycocholic acid,glycodeoxycholicacid,chenodeoxycholic acid,deoxycholic acid and muscone in Pientzehuang (Bovis Calculus,Moschus,Notoginseng Radix et Rhizoma,etc.).METHODS The analysis of methanol extract of this drug was performed on a 40 ℃ thermostatic Waters CORTECS UPLC C18column (100 mm × 2.1 mm,1.6 μm),with the mobile phase comprising of acetonitrile-water (containing 0.1％ formic acid) flowing at 0.25 mL/min in a gradient elution manner.RESULTS Thirteen constituents showed good linear relationships within their own ranges (r ＞0.998 5),whose average recoveries were 91.1％-105.3％ with the RSDs of 2.4％-4.6％.CONCLUSION This accurate,simple,sensitive and reproducible method can be used for the quality control of Pientzehuang.

Simultaneous determination of sixteen mycotoxins contaminants in cogon rootstalk by QuEChERS-UPLC-QqQ mass spectrometry / 中国中药杂志

A method for the simultaneous determination of sixteen mycotoxins in cogon rootstalk was developed using ultra-performance liquid chromatography coupled with triple quadropole mass spectrometry(UPLC-QqQ-MS/MS). The samples were extracted with acetonitrile contained 1% acetic acid and purified by QuEChERS method. The separation was performed on an Agilent Eclipse Plus C₁₈column by gradient elution using methanol and 0.01% aqueous formic acid as mobile phase. The targeted compounds were detected in MRM mode by mass spectrometry with electrospray ionization(ESI)source operated in positive ionization mode. The linear relationships of the sixteen mycotoxins were good in their respective linear ranges. The correlation coefficients(r)ranged among 0.996 2-1.000. The LOQs of the sixteen mycotoxins were between 0.03 and 186.68 μg•kg ⁻¹. The average recoveries ranged from 60.28% to 129.2% with relative standard deviations(RSDs)within 0.29%-11%. The results demonstrated that the proposed method was sensitive and accurate, and suitable for the mycotoxins quantification in cogon rootstalk.

Simultaneous determination of six bioactive constituents in Reduning Injection by UPLC-QqQ-MS/MS / 中草药

Objective: An ultra high performance liquid chromatography coupled to triple quadrupole mass spectrometry (UPLC- QqQ-MS/MS) method has been established to simultaneously determine the contents of six bioactive constituents [japonicaside A (JA), L-phenylalanion secologanin B (PSB), luteolin, scopolamine, (1S,6R,7R,10R)-6-carboxy-10-methyl-α-methylene-1-(1- oxobutyl)-cyclohexane acrylic acid (CMCA), and 3α,5α-tetrahydrodeoxycordifoline lactam (TL)] from Reduning Injection. Methods: This chromatographic separation was performed on an Agilent Zorbax SB-Aq C18 (150 mm × 2.1 mm, 3.5 μm) column with the mobile phase consisting of 0.1% formic acid water (A) and methanol (B) in a gradient elution (0.01-2.00 min, 5% B; 2.00-4.00 min, 5%-40% B; 4.00-11.00 min, 40%-95% B; 11.00-13.00 min, 95% B; 13.00-13.10 min, 95%-5% B; 13.10-14.00 min, 5% B) at a flow rate of 0.5 mL/min and the colunm temperature was set at 20℃. The analytes were detected using electrospray ionization (ESI) source by positive and negative ion monitoring mode. A triple quadrupole mass spectrometer was operated by ESI source in positive and negative ionization mode with multiple reaction monitoring for the detection of the six compounds. In the positive ion monitoring mode, the flow rate of Collision Gas (CAD) was 8 mL/min, the flow rate of Curtain Gas (CUR) was 20 mL/min, the temperature (TEM) was 500℃ and the Ion Spray Voltage (IS) was 4 500 V. In the negative ion monitoring mode, the flow rate of Collision Gas (CAD) was 8 mL/min, the flow rate of Curtain Gas (CUR) was 20 mL/min, the temperature (TEM) was 500℃ and the Ion Spray Voltage (IS) was -4 500 V. Results: All calibration curves of the six components showed excellent linear regressions (r ≥ 0.999 0) within the test range. The average recoveries were 78.93%, 114.65%, 101.99%, 90.98%, 98.08%, and 115.58%, and the average contents of six bioactive constituents in 16 batches of Reduning Injection were 2.00, 26.63, 52.63, 5.29, 34.64, and 9.69 μg/mL, respectively. Conclusion: The established method is rapid, accurate, and has high repeatability, which could provide scientific evidences for the quality control of Reduning Injection.

Effects of red ginseng saponin components on neurochemicals in rat plasma / 中草药

Objective To investigate the effects of red ginseng saponin components A and B on 15 neurochemicals in rat plasma. Methods Saponin components A and B were prepared from red ginseng total saponin by macroporous adsorption resin. The composition and contents of saponin components A and B were detected using UPLC-Q-TOF-MS/MS method. A total of 15 kinds of neurochemical substances such as dopamine (DA), adrenaline (E), norepinephrine (NE), serotonin (5-HT), 5-hydroxytryptamine (5-hydroxytryptamine), tyrosine (Tyr), glycine (Gly), glutamic acid (Glu), glutamine (Gln), aspartic acid (Asp), taurine (Tau), serine (Ser), tryptophan (Try), acetylcholine (Ach), and histamine (His) were measured by high performance liquid chromatography- mass spectrometry (UPLC-QQQ-MS/MS). Results By analyzing the intrinsic relationship between saponin composition and amount of neurochemicals, it was found that components A and B had significant differences in saponin composition, and the larger polar saponins were mainly concentrated in component A. The polar of saponin contained in B is relatively small. The levels of Ach, Tau, Glu, Gln, Asp, Tyr, E, NE, and DA in rat plasma of each dose group were increased, and the plasma levels of Gly, His, 5-HT, Ser, HIAA, and Try were significantly increased and positively correlated with the dose, suggesting that the larger polar saponins could increase the excitatory neurochemical content and the smaller saponin fraction inhibitory neurochemicals. Conclusion Red ginseng has a moderating effect on the content of central nervous system. The content of smaller polar saponins is related to the maintenance of brain activity, improvement of memory function, prevention of brain fatigue, maintenance of awakening and nervous system of anti-aging, while the larger polar saponin fraction is associated with the regulation of psychiatric rhythm, reduction of stress response and improvement of sleeping.

Determination of Donkey-hide Gelatin in Lüjiao Buxue Granules by UPLC-QQQ/MS / 中国药房

OBJECTIVE:To establish a method for the determination of donkey-hide gelatin in Lüjiao buxue granules. METH-ODS:Trypsin was used for enzymatic hydrolysis of donkey-hide gelatin. UPLC-QQQ/MS was adopted for the determination of don-key-hide gelatin in the preparation:Hypersil GOLD C18 column was used with mobile phase consisted of 0.1% formic acid solu-tion-acetonitrile(gradient elution)at the flow rate of 0.3 mL/min. The column temperature was 30 ℃,and sample size was 5 μL. Mass chromatography condition was that ion source was electrospray ion source;ionization mode was ESI+;multiple response mon-itoring was adopted,and characteristic molecular ion peaks of donkey-hide gelatin with mass-to-charge ratio of m/z 539.8(double charge)→ 612.4 and m/z 539.8(double charge)→ 923.8 were used as detection ion pair. Spray voltage was 3100 V;sheath gas was 20 Arb;auxiliary gas was 8 Arb;ion transfer tube temperature was 350 ℃;evaporation temperature was 350 ℃;scan mode was SRM. Collision gas was high purity argon. RESULTS:The sample size of donkey-hide gelatin ranged 20.24-2024 μg/mL(r=0.9978). The detection limit was 1%. RSDs of precision,stability and reproducibility tests were all lower than 6.0%. The charac-teristic molecular ion peaks of donkey-hide gelatin could be detected in 27 batches of samples. CONCLUSIONS:The method is spe-cific and can be used for the determination of donkey-hide gelatin in Lüjiao buxue granules.

Qualitative Detection of Donkey-hide Gelatin in Fufang Ejiao Buxue Granule by UPLC-QQQ/MS / 中国药师

Objective:To establish an analytical method for the identification of donkey-hide gelatin in Fufang Ejiao Buxue gran-ule.Methods:The identification of donkey-hide gelatin in Fufang Ejiao Buxue granule was established by rapid resolution liquid chro -matography (UPLC) coupled with triple quadruple mass spectrometry (QQQ-MS).Results: The characteristic molecular peaks of donkey-hide gelatin were detected in ten batches of commercial samples .Conclusion:The present method is specific , precise and reli-able, and suitable for the identification of donkey-hide gelatin in Fufang Ejiao Buxue granule .The method provides scientific reference for the study of quality control method for gelatin ingredients in Chinese patent medicines .