RESUMO
【Objective】 To study the distribution and haplotype polymorphism of HLA-A, -B, -C, -DRB1, -DQB1 alleles in Anhui Han population. 【Methods】 The HLA-A, -B, -C, -DRB1 and -DQB1 genotyping of 3 169 random unrelated stem cell donors was performed by PCR-SBT. The allele frequency, haplotype frequency and linkage imbalance parameters were calculated by counting method, maximum expectation algorithm and PyPop software. 【Results】 A total of 411 HLA alleles were detected in the population, of which 67, 143, 65, 75 and 64 alleles were detected for HLA-A, -B, -C, -DRB1 and -DQB1, respectively. The alleles with frequency >0.1 were HLA-A*11∶01, A*11∶01, A*24∶02, A*02∶01, C*01∶02, C*07∶02, C*06∶02, DRB1*09∶01, DRB1*15∶01, DRB1*07∶01, DQB1* 03∶01, DQB1* 03∶03, and DQB1*02∶01. 1426 HLA-A~HLA-B, 1 772 HLA-B~HLA-DRB1, 798 HLA-B~HLA-C, and 446 HLA-DRB1~HLA-DQB1 haplotypes were detected. The haplotypes showed linkage imbalance, and 19 of them showed strong linkage imbalance (RLD>0.80). 【Conclusion】 The frequency and haplotype distribution of HLA-A, -B, -C, -DRB1 and -DQB1 alleles in Anhui Han population were obtained. The distribution of those alleles and haplotypes have their own characteristics.
RESUMO
OBJECTIVE： To establish the method for the content determination of related substance in Terazosin hydrochloride tablets. METHODS： HPLC and principal component self-control with correction factor were adopted. The determination was performed on Agilent Zorbax Eclipse XDB C18 column with mobile phase consisted of acetonitrile-perchloric acid solution （20 ∶ 80， V/V） at the flow rate of 1.0 mL/min. The detection wavelength was set at 246 nm， and sample size was 20 μL. The column temperature was 50 ℃. The linear equations of terazosin hydrochloride， impurity A， B， C were drawn. The correction factors of each impurity related to terazosin hydrochloride were calculated by slope， and relative retention time was used to determine the position of impurities. The contents of impurity A， B and C in 3 batches of Terazosin hydrochloride tablets were determined and compared with the results of impurity control method. RESULTS： The relative retention time of impurity A， B， C was 0.39， 0.74， 2.77， respectively； the linear range of them were 0.25-3.0 μg/mL， respectively. The correction factors were 0.75， 1.09， 0.84， respectively. The detection limits were 0.35， 0.51， 0.43 ng， and the limits of quantification were 0.70， 1.02， 0.86 ng， respectively. The contents of impurity A， B and C in 3 batches of Terazosin hydrochloride tablets were 0.11％-0.13％， 0.03％ and 0.09％-0.12％； impurity B did not detected. The results are consistent with the determination of impurity control method. CONCLUSIONS： The method is simple， rapid and accurate for the content determination of related substances A， B， C in Terazosin hydrochloride tablets.
RESUMO
OBJECTIVE： To establish the quality standard for Bushen quyu granules. METHODS： TLC was used for qualitative identification of Rosa laevigata， Cuscuta chinensis， processed Fallopia multiflora and Lithospermum erythrorhizon in Bushen quyu granules. And then， the content of total polysaccharides in Bushen quyu granules was determined by UV spectrophotometry. HPLC method was used for the content determination of rutin， quercetin and hyperin in Bushen quyu granules. The determination was performed on BDS C18 column with mobile phase consisted of acetonitrile-0.08％ phosphoric acid solution （gradient elution） at the flow rate of 1 mL/min. The column temperature was 30 ℃， and detection wavelength was set at 370 nm. The sample size was 10 μL. RESULTS： TLC test sample chromatogram of 4 medicinal materials showed the same spot or fluorescence at the corresponding position with the reference substance and control medicinal materials. The linear range of glucose， rutin， quercetin and hyperin were 0.003-0.018 mg/mL， 0.225-7.20 μg/mL， 0.07-2.24 μg/mL and 1.25-39.88 μg/mL（r＝0.999 5 or 0.999 9， n＝6）. RSDs of precision， stability and reproducibility tests were all less than 3％ （n＝6）. Average recoveries were 102.2％， 101.2％， 100.9％， 101.0％ （RSD＝1.28％， 2.93％， 2.41％， 1.59％， n＝6）. Average contents were 0.46 g/g， 5.48 μg/g， 8.18 μg/g and 102.88 μg/g（n＝3）. CONCLUSIONS： Established quality standard of Bushen quyu granules is accurate and reliable， and can provide scientific reference for quality control of Bushen quyu granules.