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.

AstudyofPt-metabolitesfromanewanti-hepatomadrugmiriplatinwasimportanttomiriplatin's pharmacology research. Therefore, a method based on size exclusion chromatography-inductively coupled plasma mass spectrometry ( SEC-ICP-MS) was developed to study miriplatin and its Pt-metabolites in Beagle dog plasma. This method could be used to study total platinum concentration half-quantitatively. Compared with traditional ICP-MS direct determination, data acquired from this SEC-ICP-MS method were almost the same. By using BioSep-s2000 column, 25 mmol/L of pH 7. 2 phosphate buffer as eluent, and Pt-195 as detecting isotope, we discovered miriplatin with its four Pt-metabolites in dog plasma after intra-hepatic artery administration. The main Pt-metabolite was m2 , which associated with plasma proteins. Miriplatin in plasma did not bind with plasma proteins. According to calculation, the ratio of miriplatin/m2 first decreased rapidly, and then slowly increased to its second climax, finally slowly decreased.

OBJECTIVETo investigate the distribution of rubidium (Rb), cesium (Cs), beryllium (Be), strontium (Sr), and barium (Ba) in blood and urine in general Chinese population.

METHODSA total of 18 120 subjects aged 6~60 years were enrolled from 24 regions in 8 provinces in Eastern, Central, and Western China from 2009 to 2010 based on the method of cluster random sampling. Questionnaire survey was conducted to collect the data on living environment and health status. Blood and urine samples were collected from these subjects, and the levels of Rb, Cs, Be, Sr, and Ba in these samples were determined by inductively coupled plasma mass spectrometry. The distribution of these elements in blood and urine in male or female subjects living in different regions was analyzed statistically.

RESULTSIn the general Chinese population, the concentration of Be in the whole blood was below the detection limit (0.06 μg/L); the geometric mean (GM) of Ba in the whole blood was below the detection limit (0.45 μg/L), with the 95th percentile (P95)of 1.37 μg/L; the GMs (95% CI)of Rb, Cs, and Sr in the whole blood were 2 374(2 357~2 392) μg/L, 2.01 (1.98~2.05) μg/L, and 23.5 (23.3~23.7) μg/L, respectively; in males and females, the GMs (95%CI)of blood Rb, Cs, and Sr were 2 506 (2 478~2 533) μg/L and 2 248 (2 227~2 270) μg/L, 1.88 (1.83~1.94) μg/L and 2.16 (2.11~2.20) μg/L, and 23.4 (23.1~23.7) μg/L and 23.6 (23.3~23.9) μg/L, respectively(P<0.01, P>0.05, and P>0.05). In the general Chinese population, the GM of urine Be was below the detection limit (0.06 μg/L), while the GMs (95%CI)of urine Rb, Cs, Sr, and Ba were 854 (836~873) μg/L, 3.65 (3.56~3.74) μg/L, 39.5 (38.4~40.6) μg/L, and 1.10 (1.07~1.12) μg/L, respectively; in males and females, the GMs (95%CI)of urine Rb, Cs, Sr, and Ba were 876 (849~904) μg/L and 832 (807~858) μg/L, 3.83 (3.70~3.96) μg/L and 3.47 (3.35~3.60) μg/L, 42.5 (40.9~44.2) μg/L and 36.6 (35.1~38.0) μg/L, and 1.15 (1.12~1.19) μg/L and 1.04 (1.01~1.07) μg/L, respectively (all P< 0.01). Correlation analyses showed that there were weak correlations between blood Rb and urine Rb (r=0.197)and between blood Sr and urine Sr (r=0.180), but a good correlation between blood Cs and urine Cs (r=0.487).

CONCLUSIONThe levels of Rb, Cs, Be, Sr, and Ba in the general Chinese population are similar to those reported in other countries, and there is a significant difference in the concentration of each element among the populations living in different regions, as well as significant differences in blood Rb, urine Rb, urine Cs, urine Sr, and urine Ba between males and females.

Adolescent ; Adult ; Barium ; blood ; urine ; Beryllium ; blood ; urine ; Cesium ; blood ; urine ; Child ; China ; Female ; Humans ; Limit of Detection ; Male ; Middle Aged ; Rubidium ; blood ; urine ; Strontium ; blood ; urine ; Young Adult

OBJECTIVETo establish a method to determine total bromine in urine.

METHODDiluted urine samples were directly introduced into ICP-MS then quantized by standard curve.

RESULTTotal bromine in urine was linear within 1.0~50 mg/L with r > 0.999, When spiked at a concentration of 0.020 mg/L, 0.050 mg/L, 0.150 mg/L, the recovery was 95%~98%, intra-assay precision was 1.4% 3.2%, inter-assay precision was 3.4% to 5.0%. Urine could store in -20 °C refrigerator 3 months without any bromine loss.

CONCLUSIONUsing ICP-MS to determine the urinary total bromine, the method is fast, accurate, wide linear range of features, could meet with the requirement of Part 5 of occupational health standards guide: Method determination of chemical substances in biological materials (GBZ/T 210.5-2008), a strong competitive advantage in a wide range of survey, suitable for promotion.

Bromine ; urine ; Humans ; Mass Spectrometry

OBJECTIVETo evaluated the manganese (Mn), cobalt (Co) and molybdenum (Mo) levels in blood and urine among general population in China, and thereby to analyze their prevalent features.

METHODSFrom 2009 to 2010, a total of 18 120 subjects of general population aged 6-60 years were recruited from 24 districts in 8 provinces in eastern, central and western China mainland, by cluster random sampling method. The information about their living environment and health status were collected by questionnaire, and their blood and urine samples were also collected.Inductive coupled plasma mass spectrometry (ICP-MS) was applied to test the Mn, Co and Mo levels of blood and urine samples, and the Mn, Co, Mo distribution in blood and urine among groups of population in different ages and genders were then analyzed.

RESULTSAmong general population in China, the geometric mean (GM) of Mn concentration in blood was 8.98 µg/L. The Mn concentration in blood among males and females were separately 8.14 µg/L and 9.88 µg/L (Z = -18.84, P < 0.01). The GM of Mn concentration in urine was 0.63 µg/L. The Mn concentration in urine among males and females were separately 0.62 µg/L and 0.63 µg/L (Z = -0.67, P > 0.05). The geometric mean (GM) of Co concentration in blood was 0.194 µg/L. The Co concentration in blood among males and females were separately 0.166 µg/L and 0.225 µg/L (Z = -23.04, P < 0.01). The GM of Co concentration in urine was 0.282 µg/L. The Co concentration in urine among males and females were separately 0.260 µg/L and 0.307 µg/L (Z = -7.35, P < 0.01). The GM of Mo concentration in blood was 0.25 µg/L. The Mo concentration in blood among male and female group were separately 0.27 µg/L and 0.23 µg/L (Z = -5.03, P < 0.01). The GM of Mo concentration in urine was 27.7 µg/L. The Mo concentration in urine among males and females were 29.8 µg/L and 25.6 µg/L (Z = -6.31, P < 0.01), respectively.

CONCLUSIONThe Mn, Co and Mo levels in blood and urine varied by gender and area among general population in China, the study provided basic data evidence for the following Mn, Co and Mo biological monitoring studies in near future.

Adolescent ; Adult ; Child ; China ; epidemiology ; Cobalt ; Environmental Exposure ; Environmental Monitoring ; Female ; Humans ; Male ; Manganese ; Middle Aged ; Molybdenum

OBJECTIVETo describe the distribution of zinc (Zn) and copper (Cu) in urine samples of generalpopulation in eight provinces of China, to analyze their characteristics of distribution between different region, gender and age-cohorts, and to provide the baseline of themetabolites in the general population.

METHODSFrom 2009 to 2010, 18 120 subjects from the general population aged from 6 to 60 years old were recruited from 24 areas among 8 provinces of China mainland by random sampling. The environmental and physical condition characteristics were collected from questionnaires, and urine samples were collected at the mean time. The levels of Zn and Cu in urine were measured using ICP-MS. Data were analyzed by statistical methods to compare the distribution characteristics of Zn and Cu among populations with different ages and genders.

RESULTSTotally, the median of Cu and Zn in urine were 9.28 and 115.47 µg/L respectively; and the inter-quartile range of Cu and Zn were 2.66-16.09 and 35.32-265.15 µg/L respectively. The median of Cu in male and female were 9.90 and 8.60 µg/L (Z=-5.63, P<0.001), and Zn in male and female were 140.44 and 95.27 µg/L (Z=-14.79, P<0.001). The median of Cu among the groups aged 6-12, 13-16, 17-20, 21-30, 31-45 and 46-60 years old were 9.30, 10.14, 9.67, 9.33, 8.38 and 8.74 µg/L (χ2=70.94, P<0.001), respectively, and the median of Zn 130.83, 132.07, 139.34, 109.3, 78.74 and 109.51 µg/L ((χ2=146.00, P<0.001), respectively.There was statistically significant differences in urinary Cu and Zn levels between male and female, and among the different age groups.

CONCLUSIONThe Cu and Zn levels and distribution in urine among general population between 2009 and 2010 in China were reported in this article. These basic data in China will provide scientific and reliable reference for further scientific research.

Adolescent ; Adult ; Age Factors ; Child ; China ; Copper ; urine ; Environment ; Female ; Humans ; Male ; Middle Aged ; Sex Factors ; Surveys and Questionnaires ; Zinc ; urine

OBJECTIVETo investigate the level of zinc (Zn) and copper (Cu) in whole blood among general population from 8 provinces in China, and to analyze the characteristics of distribution among different regions.

METHODSThis cross-sectional study was performed in 8 provinces from eastern, middle and western China between 2009 and 2010, including 13 110 subjects from 24 regions, and the blood and urine samples were collected. The ICP-MS was applied to test the content of ICP-MS in blood samples, and the results were used to analyze the characteristics of contents and distributions of Zn and Cu among population from different ages, genders and regions groups.

RESULTSTotally, the mean (95%CI) contents of Cu and Zn in blood were 795 (791-799)µg/L and 3 996(3 976-4 015) µg/L, respectively. The characteristics of distribution of Cu content were as followed, the content of males were lower than it of females (male:767 µg/L; female: 822 µg/L, t = -13.302, P < 0.01). The contents of blood Cu in groups of people aging 6-12, 13-16, 17-20, 21-30, 31-45 and 46-60 years old were separately 860(853-868), 758(748-769), 734(728-734), 782(774-790), 811(795-827) and 820(815-826) µg/L. The differences showed statistical significance (F = 78.77, P < 0.01). The blood Cu content of people in eastern China (800µg/L) were also significantly higher than it in middle (774 µg/L)and western China (782 µg/L) (F = 10.94, P < 0.01). Distribution of blood Zn content showed characteristics as follows: the Zn content was higher in males than in females (male 4 085 µg/L and female 3 908 µg/L, t = 8.78, P < 0.01). The contents of blood Zn in groups of people aging 6-12, 13-16, 17-20, 21-30, 31-45 and 46-60 years old were separately 3 306 (3 261-3 350), 3 888 (3 839-3 937), 3 948 (3 902-3 994), 4 272(4 228-4 315), 4 231(4 180-4 281) and 4 250 (4 205-4 294)µg/L, which showed significant statistical differences (F = 233.68, P < 0.01). The blood Zn content of people in eastern China (3 938 µg/L) were significantly lower than it in middle (4 237 µg/L)and western China (4 105 µg/L) (F = 53.16, P < 0.01). In addition, the study also compared the relation between content of Cu and Zn and the frequency of eating seafood. The results found that the frequency of eating seafood could influence the content of Cu and Zn (Cu: F = 13.54, P < 0.01; Zn: F = 200.20, P < 0.01).

CONCLUSIONThe contents and distributions of Cu and Zn in blood differs among people from different groups in ages, genders and regions. The baseline data of this study provided reliable scientific evidence for further research.

Adolescent ; Adult ; Child ; China ; epidemiology ; Copper ; blood ; Cross-Sectional Studies ; Female ; Humans ; Male ; Middle Aged ; Young Adult ; Zinc ; blood

OBJECTIVETo evaluated the levels of arsenic (As) in blood and urine among general population in China and analyze its influencing factors.

METHODSA total of 18 120 subjects from general population aged 6-60 years were recruited from 24 districts in 8 provinces in eastern, central and western China mainland from 2009 to 2010, by cluster random sampling method. Blood samples and urine samples were collected, the information of the life-style was collected by questionnaire.Inductive coupled plasma mass spectrometry was applied to test the As level in the samples, and the distribution of As in blood and urine for different ages, genders, areas and life habits were then analyzed.

RESULTSThe geometric mean (GM) of blood As concentration among general population was 2.33 µg/L;the GM of blood As in male (2.35 µg/L) was higher than and female (2.30 µg/L) (Z = -1.42, P < 0.05); from eastern, central to western China, the blood As level were 2.94, 1.30 and 0.98 µg/L (χ(2) = 643.22, P < 0.05) , respectively; the GM in smokers (2.84 µg/L) was higher than non-smokers (2.27) (Z = -6.28, P < 0.05) ;the seafood consumer had a higher blood As level (2.59 µg/L) than people not consuming seafood (1.47 µg/L) (Z = -23.68, P < 0.05). The urine As level of the whole population was 13.72 µg/L;while its GM in male (14.10 µg/L) was higher than female (13.33 µg/L) (Z = -3.94, P < 0.05); the values from eastern, central to western China were 14.14, 16.02 and 9.57 µg/L (χ(2) = 353.89, P < 0.05), respectively;the level in smokers (16.06 µg/L) was higher than nonsmokers (13.70 µg/L) (Z = -2.63, P < 0.05); the level in seafood consumers (14.82 µg/L) was higher than people not consuming seafood (10.99 µg/L) (Z = -3.20, P < 0.05). The blood As level had a positive correlation with urine As level (correlation coefficient:0.285, P < 0.05).

CONCLUSIONThe As level in blood and urine varied by gender and area among general population in China, and related to life-styles. There was a positive correlation between As level in blood and that in urine.

Adolescent ; Adult ; Arsenic ; blood ; urine ; Child ; China ; epidemiology ; Cross-Sectional Studies ; Environmental Exposure ; Female ; Humans ; Male ; Middle Aged ; Sentinel Surveillance ; Young Adult

OBJECTIVETo evaluate the levels of lead (Pb) and cadmium (Cd) in blood and urine among general population in China, and thereby analyze their prevalent features.

METHODSA total of 18 120 subjects from general population aged 6-60 years were recruited from 24 districts in 8 provinces in eastern, central and western China mainland from 2009 to 2010, by cluster random sampling method. The blood samples and urine samples of these people were collected. The questionnaire survey was used to collect the information of the living environment and health conditions.Inductive coupled plasma mass spectrometry was applied to test the Pb and Cd levels in the samples, and the distribution of Pb and Cd in blood and urine for different ages, genders, areas and life habits were then analyzed.

RESULTSAmong the general population in China, the geometric mean (GM) of blood Pb concentration was 34.9 µg/L; the GM of blood Pb in male and female groups were 40.1 and 30.4 µg/L (Z = -28.05, P < 0.05), respectively; the GM from eastern, central and western China were 31.2, 38.8 and 58.9 µg/L (χ(2) = 1 483.33, P < 0.05) , respectively. The GM of urine Pb of the whole population was 1.05 µg/L;while the GM in male and female groups were 1.06 µg/L and 1.05 µg/L (Z = -0.73, P > 0.05) , respectively;the values from eastern, central and western China were 0.76, 2.85 and 3.22 µg/L (χ(2) = 1 982.11, P < 0.05), respectively. The GM of blood Cd concentration among general population was 0.49 µg/L; and the values in male and female group were 0.60 and 0.41 µg/L (Z = -11.79, P < 0.05) , respectively; the GM from eastern, central and western China were 0.45, 0.65 and 0.67 µg/L (χ(2) = 69.87, P < 0.05), respectively; the GM of urine Cd concentration of the whole population was 0.28 µg/L, while the GM in male and female groups were 0.29 and 0.28 µg/L (Z = -3.86, P < 0.05), respectively; the values from eastern, central and western China were 0.29,0.42 and 0.18 µg/L (χ(2) = 402.76, P < 0.05), respectively. the Spearman's rank correlation coefficient for Cd in blood and Cd in urine was 0.22, for Pb in blood and Pb in urine was 0.21. Both the correlations were statistic significant (P < 0.05).

CONCLUSIONThe Pb and Cd levels in blood and urine were relatively higher among general population in China varying by gender and area. There were positive correlations between Pb and Cd levels in blood and those in urine.

Adolescent ; Adult ; Cadmium ; blood ; urine ; Child ; China ; epidemiology ; Cross-Sectional Studies ; Environmental Exposure ; Female ; Humans ; Lead ; blood ; urine ; Male ; Middle Aged ; Sentinel Surveillance ; Young Adult