Discussion on Pharmacopoeia Standard and Drug Site of Amomi Fructus Based on Quality Investigation of Commercial Samples / 中国实验方剂学杂志

ObjectiveTo investigate the quality of Amomi Fructus in the market， and to compare the difference between the seed mass and shell， so as to provide a basis for standardizing the usage of Amomi Fructus. MethodThe properties， thin layer identification， moisture， the content of bornyl acetate were determined by the methods in the 2020 edition of Chinese Pharmacopoeia， and the ash and extract content were determined according to the collection method of the 2020 edition of Chinese Pharmacopoeia. ResultAmong the 17 batches of samples， except the content of bornyl acetate in 2 batches of Amomum longiligulare， 2 batches of A. longiligulare and A. villosum mixture was lower than the standard， the quality of other samples all met the standard of the 2020 edition of Chinese Pharmacopoeia， but there were two specifications with shell and without shell. The husk rate， volatile oil， extract and bornyl acetate contents of the seed mass and shell were tested. It was found that the content of volatile oil in three kinds of Amomi Fructus seed mass was 1.8-5.3 times that of the corresponding shell， and the content of bornyl acetate in the seed mass was 8.8-62.1 times that of the corresponding shell， but there was little difference in the extract content. ConclusionBased on the above research， it is considered that the content of bornyl acetate in A. longiligulare contained in the 2020 edition of Chinese Pharmacopoeia remains to be discussed. It is tentatively determined that the total ash content of Amomi Fructus should not be more than 10.0%， and the extract content should not be less than 15.0%. At the same time， it is suggested that when Amomi Fructus is used as medicine， the dosage of Amomi Fructus should be calculated according to the removal rate of 20%-30% of shell， and it should be crushed regardless of whether it is used in shell or not.

Dynamic changes of the main active constituents in valerian rhizome and root (Valeriana amurensis Smir. ex Kom.) during different harvest periods / Cambios dinámicos de los principales constituyentes activos del rizoma y raíz valeriana (Valeriana amurensis Smir. Ex Kom.) durante diferentes períodos de cosecha

Valeriana amurensis Smir. ex Kom. widely distributed in the northeast region of China and some region in Russia and Korea, and its underground parts (roots and rhizomes) being used to cure nervous system diseases such as insomnia. The active components including the essential oil and iridoids of underground parts were investigated in different harvest periods in order to evaluate the quality for the roots and rhizomes of V. amurensis. The content of the essential oil was obtained by hydrodistillation and bornyl acetate in the oil was quantitated by GC-EI. The iridoids, valepotriates were determined by potentiometric titration and the main component, valtrate was quantitated by HPLC-UV. The factors of biomass were considered in the determination of collection period. Statistical analysis of results showed that, the highest content of the essential oil per plant was 22.69 µl in withering period and then 21.58 µl in fruit ripening period, while the highest contents of bornyl acetate, valepotriates and valtrate per plant were 2.82 mg, 31.90 mg and 0.98 mg in fruit ripening period separately. Fruit ripening period was decided as the best harvest period for the content of active constituents and output of drug, and it would provide scientific basis for the artificial cultivation of V. amurensis.

Valeriana amurensis Smir. ex Kom. Se distribuye ampliamente en la región noreste de China y en algunas regiones de Rusia y Corea, y sus partes subterráneas (raíces y rizomas) se utilizan para curar enfermedades del sistema nervioso como el insomnio. Se investigaron los componentes activos, incluidos el aceite esencial y los iridoides de las partes subterráneas de V. amurensis en diferentes períodos de cosecha para evaluar la calidad de las raíces y rizomas. El contenido del aceite esencial se obtuvo mediante hidrodestilación y el acetato de bornilo en el aceite se cuantificó por GC-EI. Los iridoides, valepotriatos se determinaron mediante valoración potenciométrica y el componente principal, el valtrato se cuantificó por HPLC-UV. Los factores de biomasa fueron considerados en la determinación del período de recolección. El análisis estadístico de los resultados mostró que el mayor contenido de aceite esencial por planta fue de 22,69 µl en el período de marchitación y luego de 21,58 µl en el período de maduración de la fruta, mientras que el mayor contenido de acetato de bornilo, valepotriatos y valtrato por planta fue de 2.82 mg, 31.90 mg y 0,98 mg, respectivamente, en el período de maduración de la fruta por separado. Se definió el período de maduración de la fruta como el mejor período de cosecha para el contenido de constituyentes activos y la producción de droga, lo cual proporcionaría una base científica para el cultivo artificial de V. amurensis.

Simultaneous Determination of Six Effective Components in Dutong Pills by GC / 中国药师

Objective:To establish a GC method for the imultaneous determination of cinnamaldehyde, bornyl acetate, costunol-ide,dehydrocostus lactone,magnolol and honokiol in Dutong pills. Methods: The determination was performed on an HP-5 column (30 m ×0.32 mm,0.25 μm) with programmed temperature. The carrier gas was nitrogen with the flow rate of 2.0 ml·min-1. The injection volumn was 1 μl and the sample split ratio was 5:1. The inlet temperature was 280 ℃. The detector was a flame ionization detector with temperature at 300 ℃. Results:The linear ranges were 32.28-516.40 μg·ml-1for cinnamaldehyde(r=0.999 3), 27.06-433.00 μg·ml-1for bornyl acetate(r=0.999 2),25.65-410.40 μg·ml-1for costunolide(r=0.999 3),26.10-417.60 μg ·ml-1for dehydrocostus lactone(r=0.999 3),24.01-384.20 μg·ml-1for magnolol(r=0.999 0) and 18.32-293.10 μg·ml-1 for honokiol(r=0.999 4). The average recovery was 99.71%(RSD=0.67%),99.34%(RSD=1.18%),100.16%(RSD=0. 34%),100.40%(RSD=0.39%),99.32%(RSD=1.22%) and 99.58%(RSD=0.58%)(n=6),respectively. Conclusion:The method is simple,sensitive and accurate,can be used to supplement the insufficient quality control of Dutong pills.

Applications of GC-MS/MS automated mass spectral deconvolution and multi reaction monitor qualitative and quantitative analysis of volatile components of Chenxiang Huaqi Tablets / 中草药

Objective To analytically screen the volatile components from Chenxiang Huaqi Tablets (CHT) using gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) combined with automated mass spectral deconvolution, and establish the methods of multiple components contents (camphor, bornyl acetate, and patchouli alcohol) from CHT using multi reaction monitor (MRM). Methods The chromatographic column was HP-5MS (30 m × 0.32 mm × 0.25 μm). Temperature program: the initial temperature was 100 ℃, at 15 ℃/min up to 300 ℃ for 2 min. Injection port temperature was 280 ℃; Ionization methods: EI ion source with ion source temperature of 230 ℃; Quadrupole temperature was 150 ℃; Interface temperature was 280 ℃; Inject volume was 1 μl. Results A total of thirteen components were screened by automated mass spectral deconvolution soft. Under the conditions of MRM collection, camphor, bornyl acetate, and patchouli alcohol were in the range of 4.5-90 mg/mL (r = 0.999 8), 3.3-66 mg/mL (r = 0.999 8), and 2.6-51.5 mg/mL (r = 0.999 9), respectively, the ratio of each component concentration to its peak area was linear, and the average recovery (n = 6) was 101.15%, 102.64%, and 100.10% respectively; The mass fraction of 10 batches of samples were in the ranges of 0.278-0.311, 0.381-0.438, and 0.229-0.381. Conclusion The method is accurate, simple, and good repeatability. It can be used for the simultaneous determination of camphor, bornyl acetate, and patchouli alcohol in CHT, which provides a reference for the improvement of the quality of this variety.

Componentes volátiles de Eriope crassipes, Hyptis conferta, H. dilatata, H. brachiata, H. suaveolens y H. mutabilis (Lamiaceae) / Volatile compounds of analysis of Eriope crassipes, Hyptis conferta, H. dilatata, H. brachiata, H. suaveolens y H. mutabilis (Lamiaceae)

This work presents the analysis by GC-MS of volatile metabolites of six Lamiaceae from Arauca (Colombia). In stems and leaves of Eriope crassipes were determined as the most abundants: citronellic acid (53,8 percent and 66,2 percent), and methyl citronellate (15,7 percent and 14,5 percent). In the inflorescences of Hyptis conferta were identified: t-cadinol (49,4 percent), and caryophyllene oxide (13,0 percent). From leaves and flowers of Hyptis dilatata were found: delta-3-carene (11,0 percent and 0,5 por ciento), camphor (43,8 percent and 12,2 percent), bornyl acetate (3,2 percent and 25,5 percent), E-caryophyllene (12,8 percent and 22,3 percent), and palustrol (6,0 percent and 10,3 percent). In the leaves of Hyptis brachiata were recognized: E-caryophyllene (8,3 percent), alpha-humulene (19,8 percent), and germacrene D (13,0 percent). The principal compounds in leaves and flowers of Hyptis suaveolens were: alpha-phellandrene (9,4 percent and 0,4 percent), limonene (10,5 percent and 2,5 percent), 1,8-cineole (1,3 percent and 15,2 por ciento), fenchone (10,8 por ciento and tr), E-caryophyllene (26,3 por ciento and 8,0 por ciento), and germacrene D (6,7 por ciento and 14,0 por ciento). In the leaves of Hyptis mutabilis were determined: sabinene (6,6 percent) beta-elemene (6,8 percent), germacrene D (14,9 percent), beta-selinene (8,8 percent), alpha-selinene (9,1 percent), and bicyclogermacrene (6,1 percent), as the most abundants.

Este trabajo presenta el análisis por GC-MS de los metabolitos volátiles de seis Lamiaceae recolectadas en Arauca (Colombia). En tallos y hojas de Eriope crassipes se determinaron como mayoritarios: ácido citronélico (53,8 por ciento y 66,2 por ciento), y citronelato de metilo (15,7 por ciento y 14,5 por ciento). En las inflorescencias de Hyptis conferta se identificaron: t-cadinol (49,4 por ciento), y óxido de cariofileno (13,0 por ciento). En hojas y flores de Hyptis dilatata se encontraron: delta-3-careno (11,0 por ciento y 0,5 por ciento), alcanfor (43,8 por ciento y 12,2 por ciento), acetato de bornilo (3,2 por ciento y 25,5 por ciento), E-cariofileno (12,8 por ciento y 22,3 por ciento), y palustrol (6,0 por ciento y 10,3 por ciento). En las hojas de Hyptis brachiata se reconocieron: E-cariofileno (8,3 por ciento), alfa-humuleno (19,8 por ciento), y germacreno D (13,0 por ciento). Los compuestos principales en hojas y flores de Hyptis suaveolens fueron: alfa-felandreno (9,4 por ciento y 0,4 por ciento), limoneno (10,5 por ciento y 2,5 por ciento), 1,8-cineol (1,3 por ciento y 15,2 por ciento), fenchona (10,8 por ciento y tr), E-cariofileno (26,3 por ciento y 8,0 por ciento), y germacreno D (6,7 por ciento y 14,0 por ciento). En las hojas de Hyptis mutabilis se determinaron: sabineno (6,6 por ciento), beta-elemeno (6,8 por ciento), germacreno D (14,9 por ciento), beta-selineno (8,8 por ciento), alfa-selineno (9,1 por ciento), y biciclogermacreno (6,1 por ciento), como los más abundantes.

Determination of Four Components in Fresh Houttuynia cordata from Different Harvest Time with Gas Chromatography-Mass Spectrometry / 世界科学技术-中医药现代化

This study was aimed to establish a method for assay of 4-terpineol, α-terpineol, bornyl acetate and methyl-n-nonylketone in Houttuynia cordata with gas chromatography-mass spectrometry (GS/MS) for the first time in order to provide experimental evidences for its quality control. Undecylen was analyzed quantitatively. GC/MS method was used in the content determination of 4 kinds of components in Houttuynia cordata. GC conditions were that the temperature was firstly increased to 70oC for 5 min, and then 5oC·min-1 to 140oC for 5 min. Then, the temperature was increased by 10oC·min-1 to 250oC for 10 min. The temperature of the injection port was 230oC. The carrier gas was high purity helium. The flow rate was 1.0 mL·min-1. The split ratio was 10:1. The sample quantity was 1 μl. MS conditions were that the detector was MS, EI was 70ev, the temperature of four poles was 150oC, the temperature of ion source was 230oC. The results showed that there was good linearity of four components, which were 4-terpineol, α-terpineol, bornyl acetate and methyl-n-nonylketone obtained within the ranges of 6.492~129.84μg·min-1, 1.097~21.944 μg·min-1, 12.128~242.56 μg·min-1, and 84.76~169.52 μg·min-1, respectively. The average recoveries of the four components were 81.2%, 80.6%, 88.3%, and 84.6%, respectively. The RSDs were 1.5%, 2.3%, 1.1%, and 0.7%, respectively. It was concluded that the method was simple, sensitive, and easy to operate. The simultaneous measurement of multiple indexes on the component for quality evaluation of Houttuynia cordata can effectively reflect the quality of Houttuynia cordata. It can also be used in the quality assessment of fresh Houttuynia c ordate .

Determination of Camphor, Borneol and Bornyl Acetate in Shenling Baizhu Powder by Gas Chromatography / 中国中医药信息杂志

Objective To establish a GC method for simultaneous determine of camphor, borneol and bornyl acetate in Shenling Baizhu Powder. Methods Capillary column was used with 100% methyl polysiloxane as stationary phase. The temperature-programmed was as follows:starting temperature of 60 ℃, 5 ℃/min, rose to 130 ℃, kept for 5 minutes, followed by 20 ℃/min up to 230 ℃, and kept for 5 minutes. Results The average recovery rate of camphor was 99.87%, RSD was 1.3%, and good linear relationship was showed in the range of 0.003 77-0.150 8 μg (r=0.999 9). The average recovery of borneol was 100.71%, RSD was 2.1%, and good linear relationship was showed in the range of 0.002 411-0.096 4 μg (r=0.999 9). The average recovery rate of bornyl acetate was 101.95%, RSD was 1.3%, and good linear relationship was showed in the range of 0.003 02-0.121 1 μg (r=0.999 9). Conclusion The method is simple, reliable, accurate, and can effectively control the quality of Amomi Fructus in Shenling Baizhu Powder.

Determination of Bornyl Acetate in Kaiweixiaoshi Oral Liquor by Gas Chromatography / 中成药

Objective:To establish the method for determination of bornyl acetate in Kaiweixiaoshi oral liquor by gas chromatography.Methods:Naphthalene has been used as the internal standard substance in internal standard method. The GC system consisted of stainless steel column, PEG 20M as the stationary phase, nitrogen as the carrier gas, and FID as the detector.Results:Both bornyl acetate in the preparation and naphthalenet in internal standard have got satisfactory separation under the chromatographic condition. The mean recovery of bornyl acetate was 95.29%, and RSD was 0.61%.Conclusion: The method is sensitive, accurate and reproducible, and it can be used to control the quality of the preparation.

Supercritical CO_2 extraction of essential oil from Valeriana officinalis by orthogonal design / 中成药

AIM:To study the parameters of supercritical CO_2 extraction of essential oil from valeriana efficinalis by orthogonal design. METHODS: Four factors,such as extraction pressure,extraction temperature,extraction time and separation temperature were chosen by the observation of orthogonal design,each factor was assigned to three levels.Bornyl acetate content was selected as a marker in a position to determine optimal extraction. RESULTS: Pressure and temperature were the main factors in effecting the extraction of bornyl acetate,extraction time was minor factor relatively. CONCLUSION: The optimal extraction is as follow,parameters were extraction pressure:12 MPa,extraction temperature:45 ℃,extraction time:1 hour,separation temperature:35 ℃,it gave the best recoveries of essential oils and bornylacetate.