Content determination and chemometric analysis of 11 components in Xueli zhike syrup / 中国药房

OBJECTIVE To determine the contents of 11 components in Xueli zhike syrup， establish its chemometric method and provide reference for its quality control. METHODS HPLC method was established to simultaneously determine the contents of amygdalin， deapi-platycoside E， platycoside E， platycodin D3， euscaphic acid， tormentic acid， maslinic acid， corosolic acid， praeruptorin A， praeruptorin B and praeruptorin E in 12 batches of Xueli zhike syrup. The quality evaluation of 12 batches of samples was performed by chemometrics. RESULTS The 11 components had good linear relationships within their respective ranges （r≥0.999 1）； RSDs of precision， reproducibility and stability （24 h） tests were all lower than 2.00%. The average recovery rates ranged 96.90%-100.01% （RSDs were all lower than 2.00%）. Cluster analysis showed that 12 batches of samples were clustered into 3 groups. Principal component analysis showed that the first two principal components could represent 88.53% information of 11 components in Xueli zhike syrup. Partial least squares-discrimination analysis showed that euscaphic acid， amygdalin and praeruptorin A were the main potential markers affecting the quality of Xueli zhike syrup. CONCLUSIONS The established method can be used to control the quality of Xueli zhike syrup.

Amygdalin Ameliorates Liver Fibrosis through Inhibiting Activation of TGF-β/Smad Signaling / 中国结合医学杂志

OBJECTIVE@#To observe the effect of amygdalin on liver fibrosis in a liver fibrosis mouse model, and the underlying mechanisms were partly dissected in vivo and in vitro.@*METHODS@#Thirty-two male mice were randomly divided into 4 groups, including control, model, low- and high-dose amygdalin-treated groups, 8 mice in each group. Except the control group, mice in the other groups were injected intraperitoneally with 10% carbon tetrachloride (CCl4)-olive oil solution 3 times a week for 6 weeks to induce liver fibrosis. At the first 3 weeks, amygdalin (1.35 and 2.7 mg/kg body weight) were administered by gavage once a day. Mice in the control group received equal quantities of subcutaneous olive oil and intragastric water from the fourth week. At the end of 6 weeks, liver tissue samples were harvested to detect the content of hydroxyproline (Hyp). Hematoxylin and eosin and Sirius red staining were used to observe the inflammation and fibrosis of liver tissue. The expressions of collagen I (Col-I), alpha-smooth muscle actin (α-SMA), CD31 and transforming growth factor β (TGF-β)/Smad signaling pathway were observed by immunohistochemistry, quantitative real-time polymerase chain reaction and Western blot, respectively. The activation models of hepatic stellate cells, JS-1 and LX-2 cells induced by TGF-β1 were used in vitro with or without different concentrations of amygdalin (0.1, 1, 10 µmol/L). LSECs. The effect of different concentrations of amygdalin on the expressions of liver sinusoidal endothelial cells (LSECs) dedifferentiation markers CD31 and CD44 were observed.@*RESULTS@#High-dose of amygdalin significantly reduced the Hyp content and percentage of collagen positive area, and decreased the mRNA and protein expressions of Col-I, α-SMA, CD31 and p-Smad2/3 in liver tissues of mice compared to the model group (P<0.01). Amygdalin down-regulated the expressions of Col-I and α-SMA in JS-1 and LX-2 cells, and TGFβ R1, TGFβ R2 and p-Smad2/3 in LX-2 cells compared to the model group (P<0.05 or P<0.01). Moreover, 1 and 10 µmol/L amygdalin inhibited the mRNA and protein expressions of CD31 in LSECs and increased CD44 expression compared to the model group (P<0.05 or P<0.01).@*CONCLUSIONS@#Amygdalin can dramatically alleviate liver fibrosis induced by CCl4 in mice and inhibit TGF-β/Smad signaling pathway, consequently suppressing HSCs activation and LSECs dedifferentiation to improve angiogenesis.

Evaluation of the chemical profile from four germplasms sources of Pruni Semen using UHPLC-LTQ-Orbitrap-MS and multivariate analyses / 药物分析学报

Pruni Semen,the seed of several unique Prunus plants,is a traditional purgative herbal material.To determine the authentic sources of Pruni Semen,46 samples from four species were collected and analyzed.Ten compounds including multiflorin A(Mul A),a notable purative compound,were isolated and identified by chemical separation and nuclear magnetic resonance spectroscopy.Seventy-six communal components were identified by ultra-high performance liquid chromatography with linear ion trap-quadrupole Orbitrap mass spectrometry,and acetyl flavonoid glycosides were recognized as characteristic constituents.The flavonoids were distributed in the seed coat and cyanogenic glycosides in the kernel.Based on this,methods for identifying Pruni Semen from different sources were established using chemical fingerprinting,quantitative analysis of the eight principal compounds,hierarchical cluster analysis,principal component analysis,and orthogonal partial least squares discriminant analysis.The results showed that the samples were divided into two categories:one is the small seeds from Prunus humilis(Ph)and Prunus japonica(Pj),and the other is the big seeds from Prunus pedunculata(Pp)and Prunus triloba(Pt).The average content of Mul A was 3.02.6.93,0.40,and 0.29 mg/g,while the average content of amygdalin was 18.5,17.7,31.5,and 30.9 mg/g in Ph,Pj,Pp,and Pt,respectively.All the above information suggests that small seeds might be superior sources of Pruni Semen.This is the first comprehensive report on the identification of chemical components in Pruni Semen from different species.

Punica granatum and amygdalin extracts plus cobalamin combined with albendazole reduce larval burden and myositis in experimental trichinosis / Extratos de Punica granatum e amígdalina mais cobalamina combinado com albendazol reduzem a carga larvar e a miosite na triquinose experimental

Abstract Trichinellosis is a zoonosis results from eating raw or semi-cooked meat of infected animals. Medicinal plants have been used lately as alternatives and/or combined therapies to resolve some drawbacks of the current regimens. This work analyzed the effect of albendazole monotherapy on Trichinella spiralis experimental infection (group A), in comparison to P. granatum and amygdalin extracts +cobalamin (group B), plus its combination with albendazole (group C). The study revealed that the extracts alone or combined with albendazole had an inferior effect to albendazole monotherapy regarding number of adult worms (40.83 ±3.82, 18.67 ±1.86 and 16.83 ±2.32, respectively). However, their effect was more obvious in muscle phase combined with albendazole, achieving the lower number of larvae/mL tissue homogenate (22.33 ±3.27 in comparison to 39.67 ±2.58 achieved by albendazole monotherapy). The extracts exerted a significant immunomodulatory effect by reducing the local CD4+ expression in the intestine as well as in muscle phase (1.15 ±0.25 and 3.80 ±0.65 in comparison to 4.97 ±0.37 and 12.20 ±0.87 with albendazole monotherapy, respectively). So, these extracts improved the therapeutic efficacy of albendazole, specifically in muscle phase and counteracted the inflammatory reaction caused by albendazole monotherapy, thus extensively alleviating the resulting myositis.

Resumo Trichinellosis é uma zoonose resultante da ingestão de carne crua ou semicozida de animais infectados. As plantas medicinais têm sido usadas, ultimamente, como alternativas e/ou terapias combinadas, para resolver algumas desvantagens dos regimes atuais. Este trabalho analisou o efeito da monoterapia albendazole na infecção experimental por Trichinella spiralis (grupo A), em comparação com extratos de P. granatum e amígdalina +cobalamina (grupo B), além de sua combinação com albendazol (grupo C). O estudo revelou que os extratos sozinho ou combinado com albendazol teve efeito inferior à monoterapia albendazol em relação ao número de vermes adultos (40,83 ±3,82, 18,67 ±1,86 e 16,83 ±2,32, respectivamente). No entanto, seu efeito foi mais óbvio na fase muscular combinado com o albendazol, alcançando o menor número de larvas/mL homogeneizado de tecido (22,33 ±3,27 em comparação com 39,67 ±2,58 obtidos pela monoterapia albendazol). Os extratos exerceram um efeito imunomodulatório significativo, ao reduzir a expressão local CD4+ no intestino, bem como na fase muscular (1,15 ±0,25 e 3,80 ±0,65 em comparação com 4,97 ±0,37 e 12,20 ±0,87 com monoterapia albendazol, respectivamente). Assim, esses extratos melhoraram a eficácia terapêutica do albendazol, especificamente na fase muscular e neutralizaram a reação inflamatória causada pela monoterapia albendazol, aliviando extensivamente a miosite resultante.

Simultaneous determination of five ingredients in Taohe-Chengqi Decoction by UPLC-MS/MS / 国际中医中药杂志

Objective:To develop the UPLC-MS/MS method for the determination of amygdalin, cinnamic acid, rhein, emodin and glycyrrhizic acid in Taohe-Chengqi Decoction simutaneously. Methods:The separation was performed on Supelco Discovery C18, and isocratic elution was carried out with mobile phase consisting of acetonitrile - 4 mmol/L ammonium formate. The mass spectrometer was operated in the positive and negative ionization electrospray (ESI) mode using multiple monitoring (MRM) to analize of five ingredients. The precursor to product ion transitions monitored for amygdalin, cinnamic acid, rhein, emodin and glycyrrhizic acid were m/z 458.2→296.0, 146.8→103.1, 283.7→239.9, 269.7→226.1 and 821.4→350.9, respectively. Results:Amygdalin, cinnamic acid, rhein, emodin and glycyrrhizic acid were analyzed, the linear ranges were 0.001 6-0.102 4, 0.001 6-0.102 4, 0.001 6-0.102 4, 0.000 8-0.051 2 and 0.000 4-0.256 0 ng, respectively. The r were 0.998 7, 0.999 1, 0.999 5, 0.998 9 and 0.998 6, respectively. The recovery of five analytes ranges from 97.33% to 105.33% and the Relative Standard Deviations were all below 2.69%. Conclusion:This UPLC-MS/MS method is exclusive, rapid and sensitivewhich could be applied for the determination of amygdalin, cinnamic acid, rhein, emodin and glycyrrhizic acid in Taohe-Chengqi Decoction.

Discussion on Quality Control of Armeniacae Semen Amarum and Its Preparations / 中国实验方剂学杂志

Armeniacae Semen Amarum is one of the most commonly used Chinese medicinal materials， with the homology of medicine and food. It is mild toxicity， in addition to raw product， there are blazed and fried Armeniacae Semen Amarum and other processed products. The prescription， process and quality standard of Chinese herbal preparations containing Armeniacae Semen Amarum in the 2020 edition of Chinese Pharmacopoeia （volume Ⅰ）， were studied and analyzed in this paper. The quality control and safety problems of them were discussed， and the proposals were put forward：①To strengthen the quality control of medicinal materials from the origin， including processing， storage， producing area and so on. ②Production technology is the key factor affecting the safety and effectiveness of preparations， so it is necessary to strengthen the control of production process. ③To strengthen the quality research of Armeniacae Semen Amarum preparations， to develop safety quality control projects， and to further improve the quality standards of Armeniacae Semen Amarum preparations. ④To improve the safety tips of Armeniacae Semen Amarum preparations and standardize the instructions. These suggestions can provide reference for scientific understanding and evaluation of traditional Chinese medicine preparations containing Armeniacae Semen Amarum， in order to promote the quality control level of Chinese medicine preparation containing Armeniacae Semen Amarum and its processed products.

Change pattern and correlation analysis of macroscopic characteristics, active components and rancidness degrees of Armeniacae Semen Amarum in deterioration process / 中国中药杂志

To discuss the effect of deterioration on the quality of Armeniacae Semen Amarum by observing the changes of macroscopic characteristics, active components and rancidness degrees of Armeniacae Semen Amarum in deterioration process. The traditional macroscopic identification was used to observe, identify and classify the morphologic and organleptic characteristics of Armeniacae Semen Amarum. The contents of amygdalin and fatty oil(two representatives of active components) were detected by HPLC and general rule 0713 in Chinese Pharmacopoeia, respectively. Acid value and peroxide value of the samples were selected as the representative indices of different rancidness degrees, and the general rule 2303 was adopted as the method for quantitative analysis. Then principal component analysis(PCA), partial least square analysis discrimination analysis(PLS-DA) were further utilized to establish the discriminative models of samples with different rancidness degrees, and also to screen out the largest contribution factors. In sensory evaluation, Armeniacae Semen Amarum samples were divided into three groups: non-rancid, slightly-rancid, and noticeably-rancid. The color of seed coat, cotyledon and surface of noticeably-rancid samples was deepened, and the odor differed much from non-rancid samples. Average content of amygdalin and fatty oil in non-rancid samples was 4.12% and 67.77%, respectively, both meeting the requirements of Chinese Pharmacopoeia; and decreased to some extent in slightly-rancid samples. However, the content of amygdalin sharply dropped to 0.074% in noticeably-rancid samples. The acid value and peroxide value were increased significantly with the intensifying of the rancidness degree, from only 1.363 and 0.016 74 in non-rancid samples to 1.865 and 0.023 70 in slightly-rancid samples, even doubled in noticeably-rancid samples(2.167 and 0.033 82). The discriminative models established by PCA and PLS-DA could complete the task of distinguishing the non-rancid samples from noticeably-rancid ones. The contribution degree of amygdalin content as one of the input attributes of discriminative model was higher than 1. Rancidness affected the quality of Armeniacae Semen Amarum, resulting in appearance changes, decrease in content of active components, and increase in acid value and peroxide value. Obviously, noticeably-rancid samples were non-conforming to Chinese Pharmacopoeia and no longer suitable for medicinal use. Rancidness can significantly reduce the quality of Armeniacae Semen Amarum, and even could possibly produce toxicity, which should attach more attention.

HPLC fingerprint and simultaneous determination of nine components in Taohong Siwu Decoction of classical prescriptions / 中草药

Objective: To establish chemical fingerprint and multi-components determination of 15 batches of Taohong Siwu Decoction (TSD), and provide reference for the improvement of its quality control. Methods: The separation was performed on Thermo Hypersil Gold C18 column (250 mm × 4.6 mm, 5 μm) for gradient elution with methanol-0.1% phosphoric acid aqueous solution, flow rate 1.0 mL/min, column temperature 30 ℃, and detection wavelength 225 nm. The HPLC fingerprint was established and evaluated by the similarity evaluation system of TCM (version 2012A), and the difference of chemical information between 15 batches of different samples was evaluated by cluster analysis. Furthermore, the content of the nine active components in the sample was determined by HPLC multi-component wavelength switching method, with the partial least squares-discriminant analysis (PLS- DA) by SIMCA 14.1 software to find significant components of the quality between the batches. Results: The HPLC fingerprint of 15 batches of TSD was established. The similarity was greater than 0.96, and 35 common peaks were identified as gallic acid, chlorogenic acid, amygdalin, albiflorin, hydroxysafflor yellow A, paeoniflorin, ferulic acid, senkyunolide I, benzoylpaeoniflorin and ligustilide (corresponding to peaks 2, 8, 9, 13, 14, 15, 16, 25, 31, and 32). The linearity relationships of gallic acid, 5-hydroxymethylfurfural, chlorogenic acid, albiflorin, hydroxysafflor yellow A, paeoniflorin, ferulic acid, verbascoside, and senkyunolide I (r ≥ 0.999 6) were good. The results of content determination respectively were 187.5-344.4, 6.2-154.8, 413.2-459.2, 507.5-923.5, 873.8-1 202.0, 2 122.3-2 782.9, 59.2-121.3, 6.4-26.9, and 38.9-79.6 μg/g, respectively, including higher content of paeoniflorin, hydroxysafflor yellow A, and albiflorin. Furthermore, 15 batches of samples from different origins were classified into three categories. Using PLS-DA analysis, the content determination result showed that paeoniflorin, albiflorin, hydroxysafflor yellow A, and 5-hydroxymethylfurfural were the four components that affected the quality of different batches of TSD. Conclusion: HPLC fingerprint combined with multi-components determination is suitable for quality control and evaluation of TSD preparation.

Simultaneous determination of eight active components in Qingfei Decoction by HPLC and its fingerprint analysis / 中草药

Objective: To simultaneously determinate the content of chlorogenic acid, amygdalin, gardenoside, hesperidin, baicalin, wogonoside, ammonium glycyrrhizate and schisandrin in Qingfei Decoction by HPLC-VWD, and establish the fingerprint of Qingfei Decoction. The results can be applied to characterize and distinguish commercially available Qingfei Decoction preparations from different manufacturers. Methods: Agilent Technologies Zorbax SB-C18 (250 mm × 4.6 mm, 3.5 μm) column was used, with acetonitrile (A)-0.1% phosphoric acid aqueous solution (B) as the mobile phase for gradient elution, column temperature of 35 ℃, flow rate of 0.6 mL/min, injection volume of 10 μL. The content of the indicator components and the fingerprints were simultaneously assayed by the above method. Fingerprint similarity evaluation, heat map cluster analysis and other methods were used to characterize and distinguish the commercially available Qingfei Decoction preparations from different sources. Results: The specificity, linear relationship (r2 > 0.999 8), precision (RSD ≤ 1.85%, n = 6), repeatability (RSD ≤ 1.82%, n = 6), stability (RSD ≤ 1.49%, 48 h ) of eight components were good; The recovery rate of the sample was in the range of (93.19 ± 1.93)% to (102.36 ± 4.17)% (n = 6). The results of content determination showed that the daily dosage of the indicator ingredients in the marketed Qingfei Decoction preparations fluctuated greatly in different manufacturers, such as baicalin, which fluctuated from 59.85 to 224.05 mg, but the fluctuation was not obvious in different dosage forms of the same manufacturer, for example, the content of baicalin in the two preparations of KPC Herbs was 140.00 to 142.47 mg. At the same time, the similarity calculation results of fingerprints were all greater than 0.945, which indicated that the fingerprints of Qingfei Decoction from different sources were highly similar. Conclusion: The method is accurate and reliable with good repeatability. It can be used to determine the content of eight components in the commercial Qingfei Decoction preparations and establish the fingerprint of Qingfei Decoction. The commercial Qingfei Decoction preparations can be characterized by heat map clustering analysis of the daily dosage of the eight components and the fingerprint similarity evaluation to distinguish the commercially available preparations of Qingfei Decoction from different sources.

Overall quality evaluation of Fenghan Ganmao Granules based on multi- components quantitative determination and chemometric analysis / 中草药

Objective: To establish a method for the simultaneous content determination of 14 chemical components such as D- amygdalin, puerarin, hesperidin in Fenghan Ganmao Granules (FGG) by UHPLC-UV wavelength switching method, and chemometric analysis was used to analyze the quality differences. Methods: Separation was performed on an Agilent Poroshell 120 EC-C18 (150 mm × 2.1 mm, 2.7 μm) with a gradient elution of acetonitrile and 0.1% phosphoric acid. The content of 14 chemical components in 68 batches of samples from five manufacturers was determined by switching wavelength (210, 254, 310 nm). The radar chart, similarity evaluation, heat map and hierarchical clustering analysis, and principal component analysis (PCA) were used for data analysis. Results: The content of each component was as follows, D-amygdalin 0.063-3.885 mg/g, 3'-hydroxy puerarin 0.012-1.540 mg/g, puerarin 0.036-4.017 mg/g, 3'-methoxy puerarin 0.016-1.837 mg/g, puerarin-6″-O-xyloside 0.004-0.449 mg/g, mirificin 0.021-2.076 mg/g, daidzin 0.010-1.527 mg/g, prim-O-glucosylcimifugin 0.007-0.471 mg/g, 5-O-methylvisammioside 0.062-1.029 mg/g, hesperidin 0.210-8.453 mg/g, rosmarinic acid 0.001-0.237 mg/g, oxypeucedanin hydrate 0.007-0.204 mg/g, glycyrrhizic acid 0.056-1.311 mg/g, oxypeucedanin 0.002-0.042 mg/g, respectively. Chemometric analysis showed that there were some differences among the samples from different manufacturers, and the samples from the same manufacturer were more consistent. Conclusion: The method is simple, reproducible, and specific, which provides a reference method for the overall quality evaluation of FGG.

Effect of peeling on amygdalin content in Pruni semen / 国际中医中药杂志

Objective@#The present study aimed to explore the rationality of peeling process of Pruni semen through the determination of amygdalin.@*Methods@#The content of amarogentin in seed coat, seed kernel and total seed of Pruni semen, respectively, were determined by HPLC according to the methods of content determination under Pruni semen in Chinese Pharmacopeia (2015). The chromatographic column was Inertsil ODS-SP C18 (4.6 mm×150 mm, 5 μm). The gradient elution with acetonitrile-water as mobile phase was performed. The flow velocity was 0.6 ml/min, the column temperature was 40 ℃, and the wavelength was 210 nm.@*Results@#The average recovery rate (n=6) was 98.26%. The sample was stable within 24 h, and the RSD (n=6) was 1.12%. The quality of control products was good in the range of 0.02-0.40 μg. The analysis indicated that there is no significant differences (P>0.05) in the contents of amygdalin in seed coat, seed kernel and total seed of Pruni semen.@*Conclusions@#With the content of amygdalin as the index of evaluation, the Pruni semen had better not be peeled.

Simultaneous determination of six kinds of components in Buyang-Huanwu decoction by UHPLC-MS/MS / 国际中医中药杂志

Objective To develop the UHPLC-MS/MS method for the determination of amygdalin, paeoniflorin, ferulic acid, calycosin glucosidase, quercetin and formononetin in Buyang-Huanwu decoction. Methods Isocratic elution was carried out with mobile phase consisting of methanol- 2 mM ammonium formate. The separation was performed on Agilent ZORBAX SB-C18 maintained at 35 ℃. The flow rate was 200 μl/min, and the injection volume was 2 μl. The mass spectrometer was operated in the positive and negative ionization electrospray (ESI) mode using multiple monitoring (MRM) for analysis of six components. The mass spectrometric conditions were that ion source temperature 400 ℃, dry gas flow 500 L/h, atomization gas flow rate 75.8 Kpa, spray voltage 4000 V, dry gas temperature 400 ℃. Results The amygdalin, paeoniflorin, ferulic acid, calycosin glucosidase, quercetin and formononetin were all analyzed exactly, and the linear ranges were 0.5-32, 0.2-12.8, 0.1-6.4, 0.8-51.2, 0.4-25.6, 0.08-5.12 ng, respectively. The r were 0.9921, 0.9945, 0.9928, 0.9958, 0.9947, 0.9966, respectively. The recoveries of six analytes ranged from 99.21％ to 101.44％ and the relative standard deviations were all below 2.05％. Conclusions A sensitive, accuracy and suitable UHPLC-MS/MS method has been developed, and the method could be applied for the determination of amygdalin, paeoniflorin, ferulic acid, calycosin glucosidase, quercetin and formononetin in Buyang-Huanwu decoction.

Effect of peeling on amygdalin content in Pruni semen / 国际中医中药杂志

Objective The present study aimed to explore the rationality of peeling process of Pruni semen through the determination of amygdalin. Methods The content of amarogentin in seed coat, seed kernel and total seed of Pruni semen, respectively, were determined by HPLC according to the methods of content determination under Pruni semen in Chinese Pharmaсopeia (2015). The chromatographic column was Inertsil ODS-SP C18 (4.6 mm×150 mm, 5 μm). The gradient elution with acetonitrile-water as mobile phase was performed. The flow velocity was 0.6 ml/min, the column temperature was 40 , and the wavelength was ℃210 nm. Results The average recovery rate (n=6) was 98.26%. The sample was stable within 24 h, and the RSD (n=6) was 1.12%. The quality of control products was good in the range of 0.02-0.40 μg. The analysis indicated that there is no significant differences (P>0.05) in the contents of amygdalin in seed coat, seed kernel and total seed of Pruni semen. Conclusions With the content of amygdalin as the index of evaluation, the Pruni semen had better not be peeled.

Chemical components and pharmacological effects for Guizhi Fuling Prescription and predictive analysis on quality marker (Q-marker) / 中草药

Guizhi Fuling Prescription is a classic prescription for promoting blood activation and resolving stasis. It has the functions of improving blood rheology, regulating endocrine, anti-inflammation, anti-cancer, and analgesia. In ancient times, it was used to treat women’s bleeding during pregnancy, abdominal pain, and postpartum lochia. It is also often used to treat gynecological diseases in modern clinics, such as uterine fibroids, ovarian cysts, dysmenorrhea, endometriosis and so on. This paper reviewed the research progress of chemical constituents, pharmacological activities, clinical application, and quality control of Guizhi Fuling Prescription in recent years. On the basis of this, the quality markers of Guizhi Fuling Prescription are predicted and analyzed based on the “five principles” of quality markers of Chinese materia medica in order to provide reference for the study of quality control of Guizhi Fuling Prescription.

Establishment of fingerprint of Buyang Huanwu Decoction based on core-shell chromatography and its Q-Orbitrap HRMS/MS analysis / 中草药

Objective: To establish the fingerprint of Buyang Huanwu Decoction (BHD) based on core-shell column for its quality control. Methods: The extract of BHD was separated on an Agilent Poroshell 120 SB-C18 (150 mm × 4.6 mm, 2.7 μm) with a gradient elution. The mobile phase consisted of acetonitrile-0.1% formic acid. The detection wavelength was 280 nm. The similarity evaluation of 15 batches of BHD was carried out by the “Similarity Evaluation System for Chromatographic Fingerprints of TCM”. HPLC-Q-Orbitrap HRMS/MS was used to characterize the 21 chemical compounds of the extract of BHD. Results: The chromatographic fingerprints of 15 batches of BHD were generated 21 common peaks (P1-P21), belonging to all seven medicinal herbs in 38 min. Methyl quinate (P4), calycosin-7-O-β-D-glucoside (P11), calycosin-7-O-β-D-glucoside-6″-O-malonate (P13), ononin (P15), (6αR, 11αR)-9,10-dimethoxypterocarpan-3-O-β-D-glucoside (P16), isomucronulatol-7-O-β-D-glucoside (P17), calycosin (P18), formononetin (P19), (6αR,11αR)-9,10-dimethoxypterocarpan (P20), and isomucronulatol (P21) were from Astragali Radix. Succinyl adenosine (P3), 6-hydroxykaempferol-3,6-diglucoside (P5), and kaempferol-3-O-sophoroside (P10) were from Carthami Flos. Gallic acid (P2) and paeoniflorin (P9) were from Paeoniae Radix Rubra. Vanillic acid (P7) was from Angelicae Sinensis Radix. Guanoside (P1) was from Pheretima. Amygdalin (P6) and prunasin (P8) were from Persicae Semen. Ferulic acid (P12) and senkyunolide H (P14) were from Angelicae Sinensis Radix and Chuanxiong Rhizoma. A total of 21 components were identified by UHPLC-Q-Orbitrap HRMS/MS. It was the first time to establish the UHPLC fingerprint of BHD by core-shell chromatography technology. Conclusion: The method is simple and accurate with a good reproducibility and time consuming, which will provide a basis for the further research on effective constituents in BHD.

Simultaneous Determination of 7 Constituents in Xiaoshuan Enteric-coated Capsules by HPLC-wavelength Switching Method / 中国药房

OBJECTIVE： To establish a method for simultaneous determination of 7 active constituents in Xiaoshuan enteric-coated capsules， such as chlorogenic acid， amygdalin， paeoniflorin， ferulic acid， senkyunolide Ⅰ， calycosin glycoside and ligustilide. METHODS： HPLC method was adopted. The determination was performed on Agilent Eclipse Plus C18 column with mobile phase consisted of acetonitrile-0.1％ phosphoric acid （gradient elution）. The detection wavelengths were set at 326 nm for chlorogenic acid， 210 nm for amygdalin， 230 nm for paeoniflorin， 321 nm for ferulic acid， 334 nm for senkyunolideⅠ， 274 nm for calycosin glycoside and 260 nm for ligustilide. The flow rate was set at 1.0 mL/min， and the column temperature was 35 ℃. The sample size was 10 μL. RESULTS： The linear range was 1.16-34.81 μg/mL for chlorogenic acid， 1.85-55.48 μg/mL for amygdalin， 13.22-396.50 μg/mL for paeoniflorin， 13.50-405.09 μg/mL for ferulic acid， 1.75-52.51 μg/mL for senkyunolideⅠ， 2.74-82.18 μg/mL for calycosin glycoside， 7.67-230.07 μg/mL for ligustilide （r＝0.999 1-0.999 7）， respectively. The limit of quantity were 0.056， 0.103， 0.085， 0.013， 0.136， 0.184 and 0.276 μg. RSDs of precision， stability （24 h） and reproducibility tests were lower than 2.0％ （n＝6）. Average recoveries were 99.3％，98.6％，98.8％，99.7％，97.1％，97.6％ and 99.2％ （RSD＜2.0％， n＝6）. CONCLUSIONS： Established method is accurate and simple. It can be used for simultaneous determination of 7 constituents in Xiaoshuan enteric-coated capsules.

Simultaneous Determination of 6 Kinds of Constituent in Dahuang Zhechong Pills by HPLC-PDA / 中国药房

OBJECTIVE： To establish a method for amygdalin， paeoniforin， baicalin， glycyrrhizic acid， emodin and chrysophanol in Dahuang zhechong pills. METHODS： HPLC method was adopted. The determination was performed on Welchrom C18 with mobile phase consisted of methanol-0.1％ phosphoric acid （gradient elution） at the flow rate of 1.0 mL/min. The column temperature was set at 30 ℃， and the detection wavelengths were set at 210 nm （amygdalin）， 230 nm （paeoniforin， baicalin） and 250 nm [glycyrrhizic acid （calculated with ammonium glycyrrhizinate）， emodin， chrysophanol]. The sample size was 10 μL. RESULTS： The linear ranges of amygdalin，paeonifiorin，baicalin，ammonium glycyrrhizinate， emodin and chrysophanol fell within the ranges of 21.028-157.71，2.052-90.390， 34.288-257.16， 8.252 0-61.890， 3.272 0-24.540，4.768 0-35.760 μg/mL （all r≥0.999 2）. The limits of detection were 0.105 0， 0.121 0， 0.068 6， 0.082 5， 0.024 6， 0.017 9 μg/mL. The limits of quantitation were     0.263 0， 0.362 0， 0.171 0， 0.268 0， 0.065 5， 0.047 7 μg/mL. RSDs of precision， stability（12 h）and reproducibility tests were lower than 2.00％ （n＝6）. The  average  recoveries were 96.01％-100.76％ （RSD＝1.63％，n＝6）， 97.09％-101.86％ （RSD＝1.50％，n＝6）， 99.70％-101.99％（RSD＝0.82％，n＝6），96.29％-99.52％（RSD＝1.35％，n＝6）， 98.47％-102.14％ （RSD＝1.35％， n＝6） and 97.19％-99.16％（RSD＝0.69％，n＝6），respectively. CONCLUSIONS： The method is accurate， simple and reproducible for simultaneous determination of amygdalin， paeoniforin， baicalin， glycyrrhizic acid， emodin and chrysophanol in Dahuang zhechong pills.

Cyanide Toxicity of Freshly Prepared Smoothies and Juices Frequently Consumed

Aims: This study was conducted to detect the presence of cyanide in popular fruit and vegetable smoothies and juices marketed as raw and natural. Study Design: Eleven (11) popular varieties of drinks were analyzed for total cyanide (TCN). Drinks contained raw vegetables and fruits, flax seeds, whole apples with seeds, raw almond milk, and pasteurized almond milk as ingredients. Place and Study Duration: Samples were collected from health food eateries located within Las Vegas, Nevada (USA) during the summer of 2017. Methodology: Fifty milliliters (mL) of a homogenized smoothie and juice drink and 1 gram of flax seeds were subjected to the above-referenced methods for sample preparation per USEPA Methods 9012B (digestion) followed by USEPA method 9014 (colorimetry). Results: The highest TCN was detected in drinks containing raw flax seed followed by unpasteurized raw almond milk, then fresh whole apple juice. No TCN was observed in drinks that contained none of the above mentioned items (e.g. flax seed, raw almond milk) or those utilizing pasteurized ingredients. Conclusion: This study observed that TCN is present in smoothies and juices containing raw flax seeds, fresh whole apples, and/or unpasteurized almond milk. Concentrations were detected as high as 341 μg L-1 in commercially available smoothies containing vegetables, raw flax seeds, almond milk and fruits. Smoothies with vegetables, fruits, unpasteurized almond milk, and no flax seeds contained 41 ug L-1TCN, while similar smoothies with pasteurized almond milk contained negligible to 9.6 ug L-1 CN-. Unpasteurized almond milk and raw flax seeds were the major sources of TCN in drinks. With the increased demand for raw and natural foods, there is a potential sublethal exposure of TCN by consumers.

Simultaneous Determination of 5 Constituents in Xiao'er Magan Granule by HPLC-QAMS / 中国药师

Objective:To develop a method of quantitative analysis of multi-components by single marker(QAMS)for the determi-nation of five constituents(ephedrine hydrochloride,amygdalin,liquiritin, baicalin and ammonium glycyrrhizinate)in Xiao'er Magan granule. Methods:Amygdalin was used as the internal reference substance, and the relative correlation factors(RCF) of ephedrine hydrochloride,liquiritin,baicalin and ammonium glycyrrhizinate to amygdalin were calculated and evaluated. The contents of the five constituents were determined by the external standard method(ESM) and QAMS,respectively. The content results determined by the two methods were compared and the feasibility of QAMS method was verified. Results:The RCF between amygdalin and the other con-tents was 1.237,1.318,1.327 and 0.884,respectively. There were no significant differences in the results between QAMS and ESM with the relative errors less than 0.3%. Conclusion:The QAMS method is accurate and feasible for the simultaneous determination of Xiao'er Magan granule.

Simultaneous Determination of Ephedrine Hydrochloride and Amygdalin in Kangzhi Syrup by HPLC / 中国药师

Objective:To establish an HPLC method for the determination of ephedrine hydrochloride and amygdalin in Kangzhi syrup. Methods:The separation was performed on a Waters ODS2(250 mm×4.6 mm,5 μm) column. The mobile phase consisted of acetonitrile-0.2% phosphoric acid solution(containing 0.1% triethylamine) with gradient elution,the detection wavelength was at 205 nm,the flow rate was 1.0 ml·min-1,and the column temperature was 30℃. Results: Ephedrine hydrochloride and amygdalin was linear within the range of 0.169-3.380 μg(r=0.999 9)and 0.141-2.820 μg(r=0.999 7), respectively.The average recovery of e-phedrine hydrochloride and amygdalin was 98.8% and 99.1% with the RSD of 1.93% and 1.22%(n=6), respectively.Conclu-sion:The method is rapid and accurate for the simultaneous analysis of ephedrine hydrochloride and amygdalin, which can provide a reliable way for the quality control for Kangzhi syrup.