反相高效液相色谱法测定甲肝灭活疫苗中的2-苯氧基乙醇含量

目的建立反相高效液相色谱法(RP-HPLC法)测定甲型肝炎灭活疫苗中2-苯氧基乙醇的含量。方法采用C18柱,以50%乙腈为流动相,流速为1.0mL/min,检测波长为270nm,柱温为室温。以外标法测定含量。结果2-苯氧基乙醇的浓度线性范围是0.55～111μg/mL(r=0.9995),平均回收率为100.37%,RSD为1.77%。结论RP-HPLC法可用于甲型肝炎灭活疫苗中2-苯氧基乙醇的含量测定。

SPE-HPLC法测定马破伤风免疫球蛋白F(ab')_2中Triton X-100残留量

目的：建立固相萃取高效液相色谱（SPE-HPLC）法测定马破伤风免疫球蛋白F（ab’）2中灭活剂Triton X-100的残留量。方法：采用Oasis固相萃取小柱对样品进行预处理,以水和5%甲醇为淋洗剂,以甲醇为洗脱剂,收集甲醇洗脱物用于HPLC分析。采用ZORBAX Extend-C18色谱柱（4.6 mm×150 mm,5μm）,流动相为甲醇-水（80∶20）,流速1.0 mL·min-1,检测波长230 nm,柱温30℃,进样量10μL。结果：Triton X-100浓度在0.56～55.34μg·mL-1范围内,与峰面积线性关系良好（r=0.9998）;检测限（S/N=3）为2.03 ng,定量限（S/N=10）为4.06 ng;提取回收率为91.8%。结论：本方法操作简便、准确、重复性好,可用于Triton X-100的残留量测定。

Synthesis and Crystal Structure of Carvedilol

The crystal structure of the title compound carvedilol, C24H25N2O4(Mr= 406. 47), has determined by single-crystal X-ray diffraction. The crystal is mono-clinic with space group P21/c, a=9. 094(l), b= l2. 754(1), c= 18. 330(2) A, β=97. 36(1 )°, V= 2l08. 5(4) A 3, Z= 4, D.= l. 280 g/cm3, F(000) = 864, μ=O. O88mm-1 and final R= O. O368, wR(F2) = 0.0787 for reflections (I>2σ(I) ). X-ray anal-ysis reveals that the crystal is composed of a pair of enantiomer, and there are hydrogenbonds O(3) -H(3O) -N(l ) between the two enantimers. There are two planes in themolecule.