ABSTRACT
OBJECTIVE:To determine the content of urea in Urea [13C] capsules by high performance cation-exchange chroma-tography (HPCEC). METHODS:The determination was performed on Zorbax 300 SCX column with mobile phases consisting of acetonitrile-0.1% phosphoric acid (20:80,V/V) at the flow rate of 1.0 mL/min. The detection wavelength was set at 200 nm and column temperature was 35 ℃. The sample size was 20 μL. RESULTS:The linear range of urea was 0.0039-1.0030 mg/ml(r=0.9997). The limit of quantitation was 3.918 μg/mL and the limit of detection was 0.975 μg/mL. RSDs of precision,stability and repetitive test were all lower than 2.0%. The recovery ranged 99.3%-101.0%(RSD=0.67%,n=9). CONCLUSIONS:The meth-od is simple,rapid,sensitive and suitable for the content determination of urea in Urea [13C] capsules.
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OBJECTIVE:To determine the contents of citric acid in fentanyl citrate raw materials and its injection by ion chro-matography. METHODS:The determination was performed on Thermo Dionex IonPacTM AS11-HC column with mobile phase con-sisted of potassium hydroxide (gradient elution) at the flow rate of 1.0 mL/min. The column temperature was 35 ℃,and sample size was 20 μL. The detector was suppressed conductivity detector. RESULTS:The linear range of citric acid were 0.1157-74.05 μg/mL(r=0.9995). The limit of quantitation was 0.1150 μg/mL,and the limit of detection was 0.0400 μg/mL;RSDs of preci-sion,stability and reproducibility tests were all lower than 2.0%;the average recoveries were 99.6%-101.5%(RSD=0.68%,n=9). CONCLUSIONS:The method is environmentally-friendly and simple with good accuracy and precision,and suitable for the contents determination of citric acid in fentanyl citrate raw materials and injection.
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OBJECTIVE:To determine the content of acetic acid in Octreotide acetate for injection by IEC,and provide reference for the improvement of pharmacopoeia standards. METHODS:The column was Rezex ROA-Organic Acid H+ with mobile phase of 0.002 5 mol/L sulfuric acid at a flow rate of 0.5 ml/min,the detection wavelength was 210 nm,column temperature was 45℃,and in-jection volume was 100 μl. RESULTS:The linear range of acetic acid was 0.394 4 μg/ml-78.89 μg/ml(r=0.999 9);RSDs of preci-sion,stability and reproducibility tests were all lower than 2%;the limit of quantification was 197.2 ng/ml,and limit of detection was 78.89 ng/ml;recovery was 104.71%-109.78%(RSD=1.34%,n=9). CONCLUSIONS:The method is environmental and simple with good accuracy and precision,and suitable for the content determination of acetic acid in Octreotide acetate for injection.
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Objective] To sum up professor Shan Guangzhi's clinical experience for the treatment of bone metastasis of prostate cancer. [Method] From following professor Shan Guangzhi in the clinical practice and further studying his medical cases,summarizes his experience in the treatment of prostate cancer bone metastases,and sums up his academic thoughts for the treatment of the disease.[Result] Professor Shan Guangzhi thinks that deficiency of the kidney is the basic pathogenesis of bone metastases of prostate cancer,at the same time accompanied by spleen deficiency and qi-movement disturbance. To prostate cancer patients with bone metastases, pain is the most common symptom,the reason for it is that stagnation leading to pain and poor nutrition lead to pain. The treatment should focus on two aspects,both the inner treatment and the external treatment; the internal treatment regards invigorating Qi and tonifying the kidney as the basis,also pays attention to regulate spleen and stomach,dredges the body down;the external treatment regards promoting blood circulation to remove meridian obstruction as the rule,it can effectively relieve patients' pain,and cooperates with diet,as a whole to improve the quality of survival in patients. [Conclusion]Professor Shan Guangzhi's experience in the treatment of bone metastasis of prostate cancer has exact curative effect,worth learning and promotion.
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A method of on-line solid phase extraction ( SPE )-two dimensional liquid chromatography electrospary-tandem mass spectrometric method was established for the determination of Teicoplanin concentrations in human cerebrospinal fluid. Cerebrospinal fluid samples were treated by the on-line SPE treatment, and analyzed by LC-MS/MS. The chromatographic separation was performed on a Shiseido CAPCALL-PAK C18 column with gradient elution by using 25 mmol/L ammonium acetate ( pH 6. 0 )-acetonitrile as mobile phases, and the flow rate of 1 mL/min. Detection was carried out under the selected reaction monitoring ( SRM) in positive ionization mode with scopolamine hydrobromide as internal standard. Matrix-matched calibration curves with good correlation coefficients (R2=0. 9993, n=6) were obtained in the concentration range of 25-5000 μg/L. The average recoveries varied from 100. 8% to 109. 9%. The intra-and inter-day precisions were less than 6%. The method is proved to be rapid, sensitive, accurate, and suitable to determine Teicoplanin concentrations in human cerebrospinal fluid.
ABSTRACT
An on-line two dimensional liquid chromatographic (2D-LC) method was established by using an ultimate dual gradient liquid chromatography, three chromatographic columns and valve-switching technology to detect 2460A in trichoderma hazianum fermentation liquor. MF C8 column (10 mm×4. 6 mm, 5. 0 μm) was used as purification column and MG C18 column (20 mm×4. 6 mm, 5. 0 μm) was used as enriching column. Methanol and water were used as mobile phase with a gradient elution at a flow rate of 2. 0 mL/min. The sample was separated on the Thermo Hypersil GOLD C18 column (250 mm×4. 6 mm, 5. 0μm) maintained at 40 ℃ using methanol and water. The flow rate was 1. 0 mL/min and 1. 0 mL sample was injected into the 2D-LC system. The detection wavelength was 424 nm. The whole analytical time was less than 60 min. The standard curve was linear over the 2460A concentration range of 0. 0025-10. 0 mg/L(r=0. 9981, n=8). The limit of detection was calculated to be 1 . 2μg/L ( S/N=3 ) and the limit of quantification was calculated to be 2 . 5 μg/L ( S/N=10 ) . The average recoveries varied from 88 . 0% to 104 . 4%.