浊点萃取-高效液相色谱法同时测定槲寄生中3种黄酮的含量

目的采用浊点萃取法富集槲寄生中的异鼠李素-3-O-β-D-葡萄糖苷、鼠李秦素-3-O-β-D-葡萄糖苷、鼠李秦素-3-O-β-D-(6″-β-羟基-β-甲基戊二酸半酯)葡萄糖苷,并使用高效液相色谱法测定其含量。方法采用聚乙二醇辛基苯基醚(Triton X-114)作为萃取剂,色谱柱为Synergi C18柱(250 mm×4.6 mm,4μm),流动相为乙腈(A)和体积分数0.5%乙酸溶液(B)梯度洗脱,流速为1.0 mL.min-1,柱温为30℃,检测波长为358 nm。结果测得异鼠李素-3-O-β-D-葡萄糖苷、鼠李秦素-3-O-β-D-葡萄糖苷、鼠李秦素-3-O-β-D-(6″-β-羟基-β-甲基戊二酸半酯)葡萄糖苷质量浓度分别在2.093～41.86、1.200～24.00、0.861 0～17.22 mg.L-1内与峰面积呈良好线性关系;平均回收率分别为93.2%、95.6%、94.5%。结论该方法准确、灵敏,可作为槲寄生药材质量控制的有效方法。     

红花与羟基红花黄色素A大鼠体内药动学的研究

目的:研究红花和羟基红花黄色素A(hydrosafflor yellow A,HSYA)大鼠体内药动学的特征。方法:采用HPLC-UV法测定大鼠血浆中HSYA的血药浓度,应用DAS2.0求得药动学参数。结果:红花和HSYA大鼠体内药动学过程符合二室模型,其药动学参数:Cmax分别为(4.89±0.61)mg/L,(4.61±0.19)mg/L;tmax分别为(0.75±0.00)h,(0.75±0.00)h;AUC0~6分别为(7.32±0.44)mg·h·L-1,(8.68±0.93)mg·h·L-1;t1/2α分别为(0.25±0.08)h,(0.69±0.28)h;t1/2β分别为(1.21±0.36)h,(0.98±0.15)h。结论:红花在大鼠体内吸收比HSYA快,代谢比HSYA慢,表明红花中有其他成分影响HSYA的吸收和代谢。     

替加氟静脉输注给药后血液中5-FU浓度的测定

目的:建立替加氟静脉输注后血浆中活性代谢物5-FU浓度的HPLC-UV检测方法.方法:5名肿瘤病人静脉滴注替加氟4h后采集静脉血.以阿昔洛韦为内标,采用硝酸银沉淀蛋白,上清液吹干后用流动相复溶.采用Kromasil 100-5 C18柱(4.6 mm×250 mm)色谱柱,检测波长265 nm,柱温45℃,流速1.0 mL·min-1,流动相为三乙胺(0.5％,冰醋酸调pH至6.98)-甲醇(97∶3,V/V).结果:在线性范围62.5～750 ng·mL-1内低、中、高浓度5-FU的回收率分别为:88.3％、82.4％和91.6％;低、中、高浓度的批内RSD分别为:1.6％、1.8％和3.2％;批间样品RSD分别为:13.8％、13.8％和5.7％.最低检测限为31.25 ng·mL-1.结论:方法灵敏度高、稳定性好、特异性强、干扰少,可以为5-FU药代动力学和生物等效性研究提供方法.     

国产氨酚羟考酮胶囊人体生物等效性研究

目的:评价国产与进口两种氨酚羟考酮胶囊的生物等效性。方法:24名健康男性志愿者随机交叉单剂量口服2种氨酚羟考酮胶囊,采用高效液相色谱-紫外法和高效液相-质谱-质谱法分别测定血浆中对乙酰氨基酚和盐酸羟考酮的浓度。结果:受试制剂与参比制剂中对乙酰氨基酚的tmax分别为(0.75±0.48)和(0.64±0.43)h,Cmax分别为(13.45±6.13)和(13.72±5.24)mg.L-1,t1/2分别为(1.92±0.51)和(2.24±0.72)h;AUC0-tn分别为(39.55±8.34)和(39.65±8.58)mg.L-1.h,AUC0-∞分别为(42.30±8.85)和(42.95±10.11)mg.L-1.h,受试制剂的相对生物利用度为(101.56±19.43)%;而盐酸羟考酮的tmax分别为(0.86±0.34)和(0.90±0.42)h;Cmax分别为(25.81±9.54)和(22.53±7.32)μg.L-1;t1/2分别为(4.51±0.87)和(4.52±0.73)h;AUC0-tn分别为(129.67±37.27)和(116.78±41.35)μg.L-1.h,AUC0-∞分别为...     

A Stability-indicating High Performance Liquid Chromatographic Assay for the Simultaneous Determination of Atenolol and Lercanidipine Hydrochloride in Tablets

A simple, rapid, precise and accurate isocratic reversed phase stability indicating HPLC method was developed and validated for the simultaneous determination of atenolol and lercanidipine hydrochloride in commercial tablets. The chromatographic separation was achieved on phenomenex Gemini C18 (250×4.6 mm, 5 μm) column using a mobile phase consisting of acetonitrile and buffer (20 mM potassium dihydrogen phosphate pH 3.5) in the ratio of (55:45, v/v) at a flow rate of 1.0 ml/min and UV detection at 235 nm. The linearity of the proposed method was investigated in the range of 40-160 μg/ml (r(2)=0.9995) for atenolol and 8-32 μg/ml (r(2)=0.9993) for lercanidipine. Degradation products produced as a result of stress studies did not interfere with the detection of atenolol and lercanidipine and the assay can thus be considered stability-indicating.     

HPLC-UV法测定丹黄祛瘀片中黄芪甲苷的含量

目的:建立丹黄祛瘀片中黄芪甲苷的含量测定方法。方法:采用HPLC-UV,色谱柱为Kromasil C18柱(250 mm×4.6mm),流动相为乙腈-水(32∶68),流速1.0mL/min,检测波长203nm。结果:黄芪甲苷在0.066～0.330mg/mL范围内线性关系良好(r=0.9993),回收率在95.0%～105.0%之间,平均回收率为100.1%(RSD=2.0%,n=9)。结论:该法简便,快速,结果准确,重复性好,可用于控制丹黄祛瘀片中黄芪甲苷的含量。     

Validation of an HPLC-UV method for the determination of ceftriaxone sodium residues on stainless steel surface of pharmaceutical manufacturing equipments

In pharmaceutical industry, an important step consists in the removal of possible drug residues from the involved equipments and areas. The cleaning procedures must be validated and methods to determine trace amounts of drugs have, therefore, to be considered with special attention. An HPLC-UV method for the determination of ceftriaxone sodium residues on stainless steel surface was developed and validated in order to control a cleaning procedure. Cotton swabs, moistened with extraction solution (50% water and 50% mobile phase), were used to remove any residues of drugs from stainless steel surfaces, and give recoveries of 91.12, 93.8 and 98.7% for three concentration levels. The precision of the results, reported as the relative standard deviation (RSD), were below 1.5%. The method was validated over a concentration range of 1.15-6.92 μg ml(-1). Low quantities of drug residues were determined by HPLC-UV using a Hypersil ODS 5 μm (250×4.6 mm) at 50 °C with an acetonitrile:water:pH 7:pH 5 (39-55-5.5-0.5) mobile phase at flow rate of 1.5 ml min(-1), an injection volume of 20 μl and were detected at 254 nm. A simple, selective and sensitive HPLC-UV assay for the determination of ceftriaxone sodium residues on stainless steel surfaces was developed, validated and applied.     

固相萃取-高效液相色谱法测定水中残留嘧菌酯

目的建立固相萃取-高效液相色谱法分析测定水中残留甲氧丙烯酸酯类抗菌剂嘧菌酯的含量。方法样品经过固相萃取小柱净化富集后,采用Inertsil ODS-3色谱柱,乙腈-水（60∶40）为流动相,在250 nm紫外检测波长下进行高效液相色谱分析。结果嘧菌酯在0.01~1.0 mg.L-1范围内呈现良好线性（r=0.9992）。在低、中、高三个添加水平,嘧菌酯的回收率为91.5%~105.2%,相对标准偏差3.7%~8.2%。结论本法操作简便快速,可作为水中嘧菌酯含量监测的控制方法。     

丹参及丹参注射液指纹图谱的HPLC-MS研究

目的 采用HPLC－UV－MS法对丹参药材、丹参注射液中间体及丹参注射液进行指纹图谱的研究。方法 采用Alltima C18分析柱，甲醇－水－冰醋酸梯度洗脱系统，流速：1mL/min，检测波长：281nm，MS册时记录总离子流（TIC）色谱图。结果 得到分离度较好的丹参药材、中间体及注射液的HPLC－UV及HPLC－MS指纹图谱。结论为丹参药材、中间体及注射液的质量控制提供全面、可靠的依据。