ABSTRACT
A method based on HPLC-ICP-MS was established to separate the reaction products of ( ethylenediamine) palladium(Ⅱ) chloride([Pd ( en ) Cl2])and 5’-deoxyguanylic acid ( 5’-dGMP). Two reaction products were detected at pH 8. 0 with 25 mmol/L phosphate buffer solution as chromatography eluent. One was the main product with HPLC retention time of 2. 8 min, the other product’s retention time was 3.2 min. According to ESI-MS(MS/MS) study, m/z=510, 511, 512, 514, 516[M+1]+ parent ions ( abundances same to palladium isotopes) were detected. Further analysis showed that the main product was[Pd( en) ( N1-5’-dGMP) ]. However the other product was hardly to be detected by ESI-MS. By using HPLC-DAD and HPLC-ICP-MS, we found that the two reaction products had the same UV absorption spectra and palladium percentage content. Combined with other groups’research, the other reaction product was deduced as dimmer, trimer or tetramer form of[Pd( en) ( N1-5’-dGMP) ]. Further study revealed that[Pd( en) ( N1-5’-dGMP) ] was easily formed in acid solution while its polymer form was generated in alkaline solution. At pH 6. 0, [Pd(en)(N1-5’-dGMP)] was formed within 12 hours with good stability. Research also revealed that the total amount of two reaction products declined as reaction pH climbed.
ABSTRACT
A method for the simultaneous determination of 34 pesticides in sunflower oil, soybean oil and corn oil was developed. The samples were extracted and purified by a modified QuEChERS method, and then the supernatant was analyzed by on-line gel permeation chromatography-gas chromatography-mass spectrometry ( GPC-GC-MS ) . The linear range was from 0 . 01 to 0 . 2 mg/L with a good correlation coefficients ( r≥0. 9913). The average recoveries of 31 pesticides (except p,p′-DDE, p,p′-DDD, p,p′-DDT. For detail, please reference to section 3 . 6 ) ranged from 70 . 3% to 115 . 4%, 69 . 5% to 112 . 6% and 70 . 2% to 116 . 1%spiked at 0. 05 μg/g and 0. 1 μg/g with the relative standard deviations (RSDs, n=6) less than 13. 3%, 13. 5% and 12. 1% in sunflower oil, soybean oil and corn oil samples, respectively. The LODs of this method ranged from 0. 0692 to 2. 28, 0. 0559 to 2. 01 and 0. 0584 to 2. 14μg/kg (S/N=3) in sunflower oil, soybean oil and corn oil samples respectively. The convenient operation and versatility of this method are suitable for the fast screening and detection of 34 pesticide residues in sunflower oil, soybean oil and corn oil.
ABSTRACT
Objective To evaluate the effects of nail polish on measurement of pulse oxygen saturation (SpO2) by different brands of monitors in healthy volunteers.Methods Twenty healthy female volunteers were enrolled in the study.Nine fingers of each volunteer were chosen randomly,8 nails were painted 8 different colors (transparent color,red,yellow,green,blue,purple,black,white),respectively,and the left 1 nail served as blank control.SpO2 and pulse rate (PR) were measured using TuffSat Handheld Oximeter (GE) and MP70 (Philip) and PM-9800 (Mindray) monitors.SpO2 of the 9 nails monitored and the response time for SpO2 and PR were recorded.Results (1) Compared with blank control,when MP70 monitor was used,no significant change was found in each color-induced effect on the value of SpO2 obtained (P ＞ 0.05),and blue prolonged the response time for PR and SpO2 (P ＜ 0.05) ;When PM-9800 monitor was used,black could decrease the value of SpO2 measured (P ＜ 0.05),and no significant change was found in each color-induced effect on the response time for SpO2 and PR (P ＞ 0.05) ; when TuffSat Handheld Oximeter was used,green and blue could decrease the value of SpO2 monitored,and the value of SpO2 obtained was significantly lower when blue was used (P ＜ 0.05).Black,blue,purple and white could sequentially prolong the response time for PR (P ＜ 0.05),and no significant change was found in each color-induced effect on the response time for SpO2 (P ＞ 0.05).(2) For green and blue nail polish,the value of SpO2 measured with TuffSat Handheld Oximeter was significantly lower than that measured with MP70 and PM-9800 monitors(P ＜ 0.05) ; for red,yellow and green nail polish,the response time for PR obtained with TuffSat Handheld Oximeter was significantly shorter than that obtained with MP70 and PM-9800 monitors (P ＜0.05) ; for blank control group and 8 colors of nail polish,the response time for SpO2 measured with TuffSat Handheld Oximeter was significantly shorter than that measured with MP70 and PM-9800 monitors (P ＜ 0.05).For black nail polish,the value of SpO2 measured with PM-9800 monitors was significantly lower than that measured with MP70 and TuffSat Handheld Oximeter(P ＜ 0.05).Conclusion The ability for nail polish recognition and identification is different for each monitor and the color of nail polish can exert obvious effect on the value and response time for SpO2 obtained.The results of this study shows that blue nail polish-induced effect on the value of SpO2 obtained with TuffSat Handheld Oximeter is obvious,and MP70 monitor is the most stable instrument and TuffSat Handheld Oximeter is the most sensitive instrument in obtaining the value of SpO2.
ABSTRACT
Objective To investigate the water source contamination in Jiangsu Province. Methods Using blowing and arresting device and GC-MS, 90 water samples collected from 15 city drinking water sources in Jiangsu Province were analyzed. Results The main detected compounds were 1, 2-dichloroethane, chloroform, benzene, trichloroethene, toluene, tetrachloroethene, chlorobenzene, m-xylene, p-xylene, o-xylene, 1, 4-dichlorobenzene, 1, 2-dichlorobenzene, 1, 2, 4-trichlorobenzene and hexachlorobutadiene, while 1, 1-dichloroethene, trans-1, 2-dichloroethene, cis-1, 2-dichloroethene, 1, 1, 1-trichloroethane, carbon tetrachloride, bromodichloromethane, dibromochloromethane, bromoform, isopropylbenzene, 1, 2, 3-trichlorobenzene and styrene were not found. The highest concentration of 1, 2-dichloroethane was 27.79 ?g/L, which was close to the limit of surface water. It should be noticed that the detected concentrations of chlorobenzene in water source of district 3 and water source of district 4 were a little higher. Compared with the others, in water source of district 1, water source of district 9 and water source district of 14 a higher concentration of toluene and xylene were detected and the concentration of benzene in water source of district 1, water source of district 2, water source of district 3 and water source district 4 was higher. Only in water source of district 13, none of 25 volatile organic compounds was detected. Conclusion Some drinking water sources have been contaminated by volatile organic compounds in Jiangsu Province.
ABSTRACT
AIM The aim is to investigate the chemical constituents of Belamcanda chinensis. METHODS The chemical constituents were isolated and purified by solvent extraction together with various chromatographic techniques. The stuctures was elucidated on the basis of chemical evidence and spectral data. RESULTS Eight compounds were isolated from the ethanol extract of the rhizome of Belamcanda chinensis (L.)DC..Among them,six isoflavones were elucidated as irilone(Ⅰ)、genistein(Ⅱ)、tectorigenin(Ⅲ)、 irigenin(Ⅳ)、dimethyltectorigenin(Ⅴ)、irisflorentin(Ⅵ). CONCULSION ⅠandⅡ were isolated from this medicinal plant for the first time.
ABSTRACT
ObjectTo investigate the chemical constituents in the rhizoma of Belamcanda chinensis (L.) DC. MethodsThe chemical constituents were isolated and purified by solvent extraction together with various chromatographic techniques. The structures were elucidated on the basis of chemical evidence and spectral data. ResultsThree compounds were isolated from the EtoAC extracts of the rhizome of B. chinensis which were isorhamnetin (Ⅹ), hispidulin (Ⅺ), dichotomitin ( ⅩⅡ); four compounds were isolated from n-BuOH extracts, which were iridin ( ⅩⅢ), tectoridin (ⅩⅣ), daucosterol ( ⅩⅤ), vittadinoside or stigmasterol-3-O-glucoside ( ⅩⅥ). ConclusionCompound Ⅺ is isolated from this medicinal plant for the first time.