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OBJECTIVE：To establish a method for the content determination of potential genotoxic impurity maleic hydrazide in azintamide raw material. METHODS ：HPLC-FLD method was adopted. The determination was performed on Thermo Syncronis C18 column with mobile phase consisted of 0.2 mol/L acetic acid-methanol （gradient elution ）. The column temperature was set at 30 ℃，the excitation wavelength was 315 nm and emission wavelength was 389 nm. The flow rate was 1 mL/min，and the sample size was 20 μL. RESULTS：The blank solvent and azintamide did not interfere with the determination of maleic hydrazide. The linear range of maleic hydrazide was 19.5-300 ng/mL（r＝0.999 9）. The limit of detection was 4.5 ng/mL and the limit of quantification was 19.5 ng/mL. The recovery ranged from 98.79％ to 103.76％（RSDs were lower than 3.00％，n＝9）. RSDs of precision and stability （24 h）tests were no more than 5.63％，and those of durability tests were less than 2.00％（n＝6）. Maleic hydrazide was not detected in 3 batches of azinamide raw material. CONCLUSIONS ：The method is specific ，sensitive and accurate. It can be used for the trace determination of maleic hydrazide in azintamide or other matrix.
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Objective To establish a convenient and efficient method to detect Environmental endocrine disruptors (EDCs) in atmospheric particulate matter. Methods Atmospheric total suspended particles (TSP) was sampled through glass fiber filter paper in a medium-flow TSP sampler at a flow rate of 100L/min for 2 hours. The filter paper sample was then subjected to the treatments as follows: (1) The samples were extracted with acetone and dichloromethane (3:2,v/v) from glass fiber filter paper. (2) Ultrasonic cleaning for 30 minutes. (3) Centrifugation at 2,500r/min for 20 minutes. (4) The supernatant was dried out in water baths at 55℃, and then acetonitrile was added to make the volume constant. Chromatographic condition was : HPLC-FLD ( λex=275nm，λem=312nm) . Results The content of OP, NP and BPA in the standard series showed a good linear relationship with their respective peak areas, and all the correlation coefficients were greater than 0.99. The detection limits for BPA, OP, NP were 9.80 ng/ml, 5.60 ng/ml, and 5.30 ng/ml, respectively, and the recoveries were 92.10%~127.00%, 83.90%~97.40%, and 83.70%~101.20%, respectively. The RSD for the inter-and intra-day was less than 5%. Conclusion The method was simple, rapid, and accurate, which could be used for the detection of environmental endocrine disruptors in atmospheric particulate matter.
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OBJECTIVE:To develop a method for simultaneous determination of irinotecan(CPT-11)and its active metabo-lite 7-ethyl-10-hydroxycamptothecin(SN-38)in human plasma.METHODS:After precipitated by acetonitrile and acidified with hy-drochloric acid,using camptothecin as internal standard,the plasma sample was determined by HPLC-FLD. The determination was performed on Waters Luna C18column with mobile phase consisted of 0.05 mol/L sodium dihydrogen phosphate-acetonitrile(70:30, V/V,adjusted pH to 4.0 by phosphoric acid)at flow rate of 1 mL/min. The excitation wavelength was set at 380 nm;the emis-sion wavelengths of CPT-11 and SN-38 were set at 480 nm and 535 nm,respectively. The column temperature was 25 ℃ and the sample size was 20 μL. RESULTS:The linear ranges were 200-1 000 ng/mL for CPT-11(r=0.999 4,n=5)and 5-45 ng/mL for SN-38(r=0.999 2,n=5). RSDs of inter-day and intra-day were 1.68%-5.57%. The relative recoveries of CPT-11 and SN-38 were 90.12%-106.93%(RSD<8%,n=5)and 92.07%-102.56%(RSD<6%,n=5);the extraction recoveries of CPT-11 and SN-38 were 72.23%-86.56%(RSD<6%,n=5)and 71.98%-83.44%(RSD<7%,n=5),respectively. The plasma concentra-tions of CPT-11 and SN-38 in 5 patients with colon cancer were 431.13-617.19,13.97-31.89 ng/mL(1 h after intravenous drip-ping)and 398.14-584.43,11.61-29.94 ng/mL(2 h after intravenous dripping). CONCLUSIONS:The method is simple,rapid, sensitive,reproducible and suitable for the determination of plasma concentration and pharmacokinetic study of CPT-11 and its metabolite SN-38.
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OBJECTIVE:To develop a method for simultaneous determination of irinotecan(CPT-11)and its active metabo-lite 7-ethyl-10-hydroxycamptothecin(SN-38)in human plasma.METHODS:After precipitated by acetonitrile and acidified with hy-drochloric acid,using camptothecin as internal standard,the plasma sample was determined by HPLC-FLD. The determination was performed on Waters Luna C18column with mobile phase consisted of 0.05 mol/L sodium dihydrogen phosphate-acetonitrile(70:30, V/V,adjusted pH to 4.0 by phosphoric acid)at flow rate of 1 mL/min. The excitation wavelength was set at 380 nm;the emis-sion wavelengths of CPT-11 and SN-38 were set at 480 nm and 535 nm,respectively. The column temperature was 25 ℃ and the sample size was 20 μL. RESULTS:The linear ranges were 200-1 000 ng/mL for CPT-11(r=0.999 4,n=5)and 5-45 ng/mL for SN-38(r=0.999 2,n=5). RSDs of inter-day and intra-day were 1.68%-5.57%. The relative recoveries of CPT-11 and SN-38 were 90.12%-106.93%(RSD<8%,n=5)and 92.07%-102.56%(RSD<6%,n=5);the extraction recoveries of CPT-11 and SN-38 were 72.23%-86.56%(RSD<6%,n=5)and 71.98%-83.44%(RSD<7%,n=5),respectively. The plasma concentra-tions of CPT-11 and SN-38 in 5 patients with colon cancer were 431.13-617.19,13.97-31.89 ng/mL(1 h after intravenous drip-ping)and 398.14-584.43,11.61-29.94 ng/mL(2 h after intravenous dripping). CONCLUSIONS:The method is simple,rapid, sensitive,reproducible and suitable for the determination of plasma concentration and pharmacokinetic study of CPT-11 and its metabolite SN-38.
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@#To evaluate pharmacokinetic and metabolic characteristics of clevidipine butyrate lipid microspheres(CDB-LM)injection in mice, a novel HPLC-FLD method was developed for simultaneous measurement of clevidipine butyrate(CDB)and its metabolites clevidipine acid(MI)in whole blood samples. The chromatographic column was Waters C18(4. 6 mm×150 mm, 5 μm)and the mobile phase is consisted of acetonitrile-methanol-phosphate(2 ∶1 ∶2). The detection wavelength of FLD included excitation wavelength at 358 nm and emission wavelength at 440 nm. The pharmacokinetic parameters of CDB and MI were calculated by using DAS 2. 0. Then obtained parameters were statisticaly analyzed using PASW Statistics 18. The results showed that the half-life of CDB and MI were about 4 min and 20 min, respectively. Pharmacokinetic parameters of the low- and high-dose groups were as follows: CL of CDB were 4. 21 and 2. 72 L ·min-1 ·kg-1; AUC0-t were 3. 86 and 6. 43 mg/L ·min; MRT0-t were 7. 09 and 6. 17 min. CL of MI were 0. 34 and 0. 22 L ·min-1 ·kg-1; AUC0-t were 52. 23 and 74. 90 mg/L ·min; MRT0-t were 201. 24 and 217. 33 min. A method of protein precipitation was established, and acetonitrile was used to deal with whole blood samples. This method was simple, fast, with no interference with endogenous impurities. The results showed that the established HPLC-FLD method was simple and sensitive. It can be used to determine CDB and MI simultaneously. Comparing the low-dose group with the high-dose group, it was found that the plasma concentration-time curve of the two groups revealed the same tendency, which confirms that CDB has a short half-life and that it metabolizes to MI quickly.
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This study aimed to determine the occurrence of AFM1 contamination in the samples of grated parmesan cheese marketed in the Metropolitan Region of Rio de Janeiro -Brazil. Thirty samples representing 10 major brands marketed in the region were analyzed by High Performance Liquid Chromatography with fluorescence detection (HPLC-FLD) after purification with immunoaffinity column. The method showed recovery values within the range of 70-90%, with RSD lower than 15% and limits of detection and quantification below the maximum level allowed by the European Commission for the presence of AFM1 in cheeses. The mycotoxin was identified in 18 (60%) of the grated cheese samples tested. The highest value corresponded to 0.69 ± 0.02 µg/kg and the mean for all the analyzed samples was 0.16 µg/kg. All the samples were lower than the limit established by the Brazilian legislation (2.5 µg/kg) for AFM1 in cheeses in general. However, eight samples (26.7%) presented AFM1 levels above the tolerance limit of 0.25 µg/kg adopted by the European Commission. These results indicated that AFM1 levels in the grated cheese consumed in Rio de Janeiro -Brazil were relatively high and it could provide a potential hazard for the public health.
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Objective:To establish a method for detecting the content of vitamin B2 in Weimeisu tablets by HPLC-FLD. Methods:A PAK C18(250 mmID × 4. 6 mm,5 μm) column was employed with methanol -0. 02 mol·L-1 ammonium acetate (35∶65) as the mobile phase, the flow rate was 1. 0 ml·min-1, and the injection volume was 10 μl. The detection wavelength λex and λem were 450mn and 522 mn, respectively. Results:Vitamin B2 was linear within the range of 1.0-20 μg·ml-1(r=0.999 9). The average recovery was 99. 20%(RSD=0. 63%, n=6). Conclusion:The method is specific, sensitive and accurate, and can be used to deter-mine vitamin B2 in Weimeisu tablets.
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Two analytical methods for the determination and confirmation of ochratoxin A (OTA) in green and roasted coffee samples were compared. Sample extraction and clean-up were based on liquid-liquid phase extraction and immunoaffinity column. The detection of OTA was carried out with the high performance liquid chromatography (HPLC) combined either with fluorescence detection (FLD), or positive electrospray ionization (ESI+) coupled with tandem mass spectrometry (MS-MS). The results obtained with the LC-ESI-MS/MS were specific and more sensitive, with the advantages in terms of unambiguous analyte identification, when compared with the HPLC-FLD.