2.Determination of cyclohexanone concentration in the plasma separator by gas chromatography.
Min-Ju HUANG ; Lin YAN ; Yan-Ying HE ; Wei-Cong LIN
Chinese Journal of Medical Instrumentation 2009;33(5):381-382
This essay is to determine the cyclohexanone concentration of the plasma separator. The compound was introduced into the GC analytical system by the carrier gas. The determination was performed by the measurement of their peak area and by the external standard method.
Chromatography, Gas
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methods
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Cyclohexanones
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analysis
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Plasma
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Plasmapheresis
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instrumentation
4.Risk assessment and risk control for occupational exposure to chemical toxicants from an isophorone nitrile device.
Dejun WANG ; Xiaokuan FU ; Fanling KONG ; Shaofeng SUI ; Yuanyuan JIANG ; Yinglin DU ; Jingyang ZHOU
Chinese Journal of Industrial Hygiene and Occupational Diseases 2014;32(6):477-480
OBJECTIVERisk assessment and risk control for occupational exposure to chemical toxicants were performed on an isophorone nitrile device with an annual production of 5,000 tons, based on improved Singaporean semi-quantitative risk assessment method, with consideration of actual situation in China and in the present project.
METHODSWith the use of engineering analysis and identification of occupational hazards in the improved Singaporean semi-quantitative risk assessment method, hazard rating (HR) and risk assessment were performed on chemical toxicants from an isophorone nitrile device with an annual production of 5,000 tons.
RESULTSThe chemical toxicants in the isophorone nitrile device were mainly isophorone, hydrocyanic acid, methanol, phosphoric acid, sodium hydroxide, and sodium cyanide; the HR values were mild hazard (2), extreme hazard (5), mild hazard (2), mild hazard (2), moderate hazard (3), and extreme hazard (5), respectively, and the corresponding exposure rating (ER) values were 2.09, 2.72, 2.76, 1.68, 2.0, and 1.59, respectively. The risk of chemical toxicants in this project was assessed according to the formula Risk = [HR×ER](1/2). Hydrocyanic acid was determined as high risk, sodium hydroxide and sodium cyanide as medium risk, and isophorone, methanol, and phosphoric acid as low risk. Priority in handling of risks was determined by risk rating. The table of risk control measure was established for pre-assessment of occupational hazards.
CONCLUSIONWith risk assessment in this study, we concluded that the isophorone nitrile device with 5,000 ton annual production was a high-occupational hazard device. This device is a project of extreme occupational hazard. The improved Singaporean semi-quantitative risk assessment method is a scientific and applicable method, and is especially suitable for pre-evaluation of on-site project with no analogy.
Cyclohexanones ; Humans ; Nitriles ; Occupational Exposure ; prevention & control ; Risk Assessment
5.A new selaginellin derivative from Selaginella pulvinata.
Yuan CAO ; Yong-Ping WU ; Jin-Ao DUAN
Acta Pharmaceutica Sinica 2015;50(2):199-202
Abstract: A new selaginellin derivative named as selaginellin S (1) was isolated from the whole plants of Selaginella pulvinata (Hook. et Grev.) Maxim. (Selaginellaceae), together with a known one (selaginellin M, 2). Compounds 1 and 2 were separated and purified by silica gel and Sephadex LH-20 column chromatography. Their structures were determined on the basis of extensive spectroscopic analysis including IR, MS, 1D and 2D NMR experiments, as well as ECD calculations. Compound 1 is a key intermidiant in the biosynthesis pathway of selaginellins. Compound 2 is first reported in this plant.
Biphenyl Compounds
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chemistry
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isolation & purification
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Cyclohexanones
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chemistry
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isolation & purification
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Molecular Structure
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Selaginellaceae
;
chemistry
6.Determination of residual cyclohexanone in disposable infusion set by gas chromatography.
Li ZHANG ; Yan WEN ; Tao HE ; Minzhu WANG ; Pinghua XU
Chinese Journal of Medical Instrumentation 2014;38(5):381-385
An effective GC method was established for contents determination of the residual solvent of cyclohexanone in infusion sets for single use. The cyclohexanone in infusion sets for single use products were extracted with circular pump, using ethylalcohol as the extraction solven, then the extract followed by analysis of gas chromatography-tandem mass spectrometry. The method was simple, rapid, sensitive and accurate, Cyclohexanone showed good linearity in the range of (5.5-190.9) μg/mL, the correlation coefficient was 0.999 0, the detection limit (S/N = 3) was 0.133 μg/mL and limits of quantitation (S/N = 10) was 1.33 μg/mL. The spiked average recoveries ranged from 98% to 99%. The relative standard deviations (RSDs) of the method ranged from 1.03% to 1.98%. The method was simple, fast, sensitive and accurate, and may serve as a mass control method for residual cyclohexanone in disposable infusion sets for single use.
Cyclohexanones
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analysis
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Disposable Equipment
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standards
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Gas Chromatography-Mass Spectrometry
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Solvents
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analysis
8.Determination of Plasticizer DEHP Released from Medical Injection Equipment.
Jian ZHENG ; Minzhu WANG ; Wang ANYAN ; Pinghua XU ; Yin HAN ; Yan WEN ; Li ZHANG
Chinese Journal of Medical Instrumentation 2015;39(6):451-453
To established an effective GC-MS /MS method for the contents determination of the residual DEHP in injection equipment, and investigate the effect of the pretreatment on the measurement. To simulate the clinical conditions of use, under the condition of 37 degrees C balance extraction, extract liquor by chloroform extraction, then the extract followed by analysis of GC-MS /MS. The method was simple, rapid, sensitive and accurate. The limits of quantitation (LOQ, S/N = 5) of cyclohexanone was 0.075 μg/mL, The spiked average recoveries ranged from 92% to 98%. The relative standard deviations (RSDs) of the method ranged from 1.01% to 1.61%, The method was simple, fast, sensitive and accurate, and may serve as a mass control method for residual DEHP in injection equipment.
Cyclohexanones
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chemistry
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Diethylhexyl Phthalate
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chemistry
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Equipment Contamination
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Gas Chromatography-Mass Spectrometry
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Injections
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instrumentation
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Limit of Detection
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Plasticizers
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chemistry
9.Simultaneous determination of selaginellins and biflavones in Selaginella tamariscina and S. pulvinata by HPLC.
Yuan CAO ; Yongping WU ; Xiaowen ZHOU ; Fang QIAN ; Huijia FAN ; Qiang WANG
China Journal of Chinese Materia Medica 2012;37(9):1254-1258
OBJECTIVETo establish a HPLC-DAD model for the simultaneous determination of two selaginellins (selaginellin and selaginellin B) and four biflavones (amentoflavone, sequoiaflavone, hinokiflavone and isocryptomerin) contained in 10 batches of Selaginella tamariscina and 12 batches of S. pulvinata produced in different areas.
METHODThe analysis was performed on a Waters Cosmosil C18 column (4.6 mm x 250 mm, 5 microm) eluted with acetonitril-0.1% formic acid as mobile phase in a linear gradient mode. The detection wavelength was set at 280, 337 nm. The flow rate was kept at 1.0 mL x min(-1), and the column temperature was 30 degrees C.
RESULTThe six active constituents showed significant different in content. Amentoflavone in S. tamariscina contains (5. 628-9. 184 mg x g(-1)) is more than that contained in S. pulvinata (0.823-7.131 mg x g(-1)), while selaginellin in S. pulvinata (0.123-0.593 mg x g(-1)) is more than that contained in S. tamariscina (0.067-0.133 mg x g(-1)). All the calibration curves showed good linear correlation coefficients (r > 0.9997) over the wide test ranges.
CONCLUSIONThe developed HPLC-DAD method is simple, sensitive and accurate and has the good repeatability in separation, which is available for the quality control of S. tamariscina and S. pulvinata.
Biflavonoids ; chemistry ; Biphenyl Compounds ; chemistry ; Chromatography, High Pressure Liquid ; methods ; Cyclohexanones ; chemistry ; Flavones ; chemistry ; Flavonoids ; chemistry ; Selaginellaceae ; chemistry
10.Study on chemical constituents from cultivated Gynura nepalensis.
Yao LU ; Zhi-Hong LI ; Lin MA ; An-Jun DENG ; Feng WU ; Zhi-Hui ZHANG ; Hai-Lin QIN
China Journal of Chinese Materia Medica 2014;39(19):3777-3781
Taking application of some isolation and purification technologies, such as solvent extraction, preliminary solvent isolation, column chromatographies over silica gel and Sephadex LH-20 gel and preparative HPLC, 10 compounds were obtained from Gynura nepalensis cultivated in the suburban area of Beijing. Their structures were identified by spectroscopic methods and comparison with literature as (3R) -3-hydroxy-β-ionone (1), (3S,5R, 6S, 7E) -5, 6-epoxy-3-hydroxy-7-megastigmen-9-one (2), (+) -boscialin (3), 3, 6-trans-3-hydroxy-α-ionone (4), 3, 6-cis-3-hydroxy-α-ionone (5), 3, 4-cis-3, 4-dihydroxy-β-ionone (6), ethyl caffeate (7), loliolide (8), 1H-indole-3-carbaldehyde (9), and 3-(hydroxyacetyl)indole (10), respectively. All compounds were isolated from the title plant for the first time, and with compounds 1, 2, 4-7, 9 and 10 being isolated from Gynura species for the first time. Structurally, the above compounds 1-6 belong to C13 nor-sesquiterpenoids, sharing the same carbon skeleton of megastigmane. According to this study, they are one of major kinds of chemical constituents of Gynura nepalensis and have important reference value for the investigation on phytotaxonomy of this species.
Asteraceae
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chemistry
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Caffeic Acids
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chemistry
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Cyclohexanones
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Drugs, Chinese Herbal
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chemistry
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Glucosides
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Indoles
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chemistry
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Mass Spectrometry
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Molecular Structure
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Norisoprenoids
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chemistry