AIM: To determine 5 different aphrodisiacs,including apomorphine,yohimbine,vardenafil,sildenafil and alprostadil,adulterated into Chinese proprietary medicine by LC/MS(n),and build a laboratory library including MS(n) spectra and retention time. METHODS: ZORBAX SB C_18 column(150 mm?4.6 mm,5 ?m)was applied.The mobile phase consisted of acetonitrile and 0.5% formic acid changing by linear gradient elution,and the flow rate was 1.0 mL/min.The ion trap mass spectrometer with positive ion mode electrospray(ESI?) was applied. RESULTS: In the mass spectrum apomorphine,yohimbine,vardenafil and sildenafil showed abundant pseudomolecular ion +,and alprostadil showed abundant pseudomolecular ion -.All the MS(n) spectra showed characteristic product ion. CONCLUSION: It is proved that the method is simple,reliable and suitable to determin aphrodisiac adulterated to health food.

AIM:To establish a specific method for the identification of 26 chemical drugs added illegally into analgesic-antipyretic traditional Chinese medicines and health food. METHODS: The liquid chromatography-ion trap mass spectrometry method was used.Comparing with retention time and spectrums of references in library set up by ourselves,the target compounds in sample were screened and identified. RESULTS: Sixty samples were tested and Naproxen,Ibuprofen and Aspirin were detected out. CONCLUSION: The method is accurate,sensitive and easy to operate, which is first reported in China and so many compounds could be detected at the same time.

Quality control of traditional Chinese medicine (TCM) has become bottlenecks of TCM industry devel-opment and TCM international recognition. To solve the retational problems, we explored the establishment of new quality control method based on efficacy and safety. Firstly, material basis of TCM efficacy was investigated deeply and systematically. Then, quality control method based on efficacy was established by using active ingre-dients as markers. We also establish detection methods based on safety, such as pesticide residues, heavy metals and harmful elements , mycotoxins .

The drugs such as sildenafil adulterated in herbal products and dietary supplements may endanger human health. The number of the new modified derivatives is increasing recently. Based on Q-TOF-MS, a new sildenafil analogue was found. It was isolated and purified by preparative liquid chromatography. Its structure was determined by NMR, as 1-[4-propoxy-3-(6, 7-dihydro-1-methyl-7-oxo-3-propyl-1H-pyrazolo[4, 3-d] pyrimidin-5-yl)phenylsulfonyl]-4-methylpiperazine. Compared with sildenafil, the ethoxy group of the benzene ring moiety was moved to the propoxy group, which had not been reported in China. The mass spectrometric behavior pattern of the structure type was summarized, which can greatly accelerate the structural analysis of novel analogues.
Chromatography, High Pressure Liquid ; Dietary Supplements ; analysis ; Drug Contamination ; Magnetic Resonance Spectroscopy ; Molecular Structure ; Piperazines ; chemistry ; isolation & purification ; Sildenafil Citrate ; chemistry ; Spectrometry, Mass, Electrospray Ionization

Objective To ascertain the concentrations of uranium in drinking water around nuclear power plants.Methods A total of 106 water samples were collected from June 2009 to March 2010 in Jiangsu,Zhejiang,Liaoning and Shandong provinces.Inductively coupled plasma-msgs spectrometry(ICPMS)was applied to determine uranium content in local water source and drinking water.The detection limit of U was 0.8 ng/L.The recovery was 100.9%.Results The uranium concentrations in all samples were less than 15μg/L which was the limit given by World Health Organization(WHO).Conclusions The concentration of uranium in water sources was as follows:Liaoning>Shandong>Jiangsu>Zhejiang.The concentration of uranium in drinking water W88 maximal in Shandong Province and minimal in Zhejiang Province.

Objective To ascertain the uranium isotopic ratios in surface water samples around nuclear power plants.Methods Water samples were collected in Jiangsu,Shandong and Zhejiang provinces.An efficient separation procedure for the trace uranium concentrated from surface water by tributyl phosphate (TBP) was used.Inductively coupled plasma mass spectrometry (ICP-MS) was applied to determination of low abundance uranium isotopes.Results The 234 U/238 U isotope ratio varied from 4.575 × 10-5to 7.752 × 10-5 and 235U/238U from 7.273 × 10-3 to 7.639 × 10-3.Conclusions The 234U is enriched in the surface water.

Objective To ascertain the uranium concentrations and uranium isotopic ratios in drinking water in Xilingol League,the Inner Mongolia Autonomous Region.Methods Drinking water samples were collected in Xilingol League,the Inner Mongolia Autonomous.Region inductively coupled plasma mass spectrometry (ICP-MS) was applied to determine the concentration of uranium and uranium isotope abundance.Results The uranium concentrations in all samples were in the range of 2.73-18.9μg/L,with an average of 8.20 μg/L.Tbe234U/238U isotope ratio varied from 7.513 × 10-5to 3.003 × 10-4 and235U/238U from 7.196 × 10-3 to 7.391 × 10-3.The relative standard deviation (RSD) was less than 0.5％ for234U/238U and 0.2％ for235 U/238U.Conclusions The uranium concentration in samples collected from Dongwuqi was high than 15 μg/L,whih is the limit given by World Health Organization (WHO).The uranium in drinking water originates from the natural environment.The234U is enriched in drinking water.

The drugs such as sildenafil adulterated in herbal products and dietary supplements may endanger human health. The number of the new modified derivatives is increasing recently. Based on Q-TOF-MS, a new sildenafil analogue was found. It was isolated and purified by preparative liquid chromatography. Its structure was determined by NMR, as 1-[4-propoxy-3-(6, 7-dihydro-1-methyl-7-oxo-3-propyl-1H-pyrazolo[4, 3-d] pyrimidin-5-yl)phenylsulfonyl]-4-methylpiperazine. Compared with sildenafil, the ethoxy group of the benzene ring moiety was moved to the propoxy group, which had not been reported in China. The mass spectrometric behavior pattern of the structure type was summarized, which can greatly accelerate the structural analysis of novel analogues.

Objective The levels of Thl cytokines(IL-10 and IL-13)and Th2 cytokines(INF-? and TNF-?)were determined in the sera of patients with Schistosomiasis japonica in order to find the relationship between cytokines and severe hepatic fibrosis(HF)in schistosomiasis.Methods A total of 358 patients with advanced Schistosomiasis japonica were examined by ultrasound.68 HBsAg negative patients were chosen randomly as experimental control.Among them,39 patients were found to have mild HF and 29 were severe HF.The sera levels of Thl and Th2 cytokines were determined with ELISA.Results Among these 358 patients,83(23.2%)were HBsAg positive.Neither earlier nor severer hepatic fibrosis was noted in the patients who had been simultaneously infected with HBV than those only infected with schistosomiasis. There was a significant difference between mild[ 1.60(1.30-12.14)ng/L]and severe[ 4.20(1.43- 52.07)ng/L]HF patients in the level of IL-10(Z=-3.907,P0.05)was found in level of IFN-?,between severe[3.12(1.38-66.14)ng/L]and mild[5.87(1.33-216.33)ng/ L]HF subjects.Our observation did not reveal any obvious difference of TNF-? between severe[ 2.48(0.79 -19.86)ng/L]and mild[ 2.28(0.67-15.72)ng/L]HF groups.Conclusions Patients infected with advanced shistosomiasis may become more susceptible to HBV.The results of the present investigation showed that a high level production of IL-13 was associated with severe HF.

Objective To explore the operative methods and clinical outcomes in emergency or sube- mergency repair for the complicated tissue defects in hand in first stage applying microsurgical technique. Methods From Jan.,2000 to Aug.,2005,49 emergency cases of complicated hand tissue defects were re- paired in the first stage with replantation,reconstruction,free flaps,combined finger reconstruction and flap transplantation,including 21 cases in mini tissue mass replantation or reconstruction,15 cases in replantation combined with free flap transplantation,8 cases in replantation and reconstruction combined with free flap transplantation,5 cases in combined multiple digits reconstruction with free flap transplantation.The free flap transplantation included the anterolateral femoral flap,the latissimus dorsi myocutaneous flap,the dorsalis pe- dis flap,the media pedis flap and the instep flap.Results All the flaps,the replanted and reconstruceted finger survived uneventfully except for one replanted finger necrosis.45 cases healed in the first stage and the other 4 cases healed in the second stage.During a follow-up from 6 months to 3 years postoperatively,a satis- factory appearance and function of the reconstructed hand was achieved.The excellent and good rate was 85.7% assessed with provisional functional assessment criterion for upper limbs issued by Chinese Society of Hand Surgery.Conclusion The emergency or subemergency repair for the complicated tissue defects in hand has the advantage of short-term treatment and desirable functional outcome.The emergency replantation and reconstruction combined with various flaps or tissue mass can be applied to repair tissue defect in hand in the first stage according to the position and area of the defect along with the technique level of the surgeon, having been proved to achieve desirable clinical outcomes.And the key points leading to a successful operation is the correct treatment for the raw surface of the defects,suitable choice for various flaps,logical design of combination pattern and prevention and timely treatment for vessel crisis.