Handling of biological samples in the determination of the anti-neoplastic drug mitomycin C

A study to ascertain suitable conditions for handling biological samples from patients, treated with the antibiotic mitomycin C (MMC), with the objective of improving the accuracy and reliability of the determination is described. Situations frequently occurring in medical practice are simulated to optimize procedures for reliable and reproducible sampling, sample treatment and determination of MMC. Continuation of drug partitioning in whole blood after sampling can be prevented by immediate cooling in ice before the separation of plasma from cells. The adjustment of the pH of urine samples is shown to be particularly important since a low urinary pH causes decomposition of MMC; moreover, it may decrease extraction recovery. Furthermore, long-term exposure of samples to daylight induces drug decomposition. Frozen storage of plasma and urine samples for periods greater than 3 weeks is to be avoided as this results in a considerable drop in MMC concentration. Repeated cycles of freezing and thawing are shown to have no effect upon the analytical results (6 cycles tested). The analysis of extracts of biological samples may take place up to at least 24 h after their preparation without measurable loss of analyte.     

Direct quantitation of antiseptic quaternary ammonium compounds by fast atom bombardment mass spectrometry

The medicinally important quaternary ammonium salts benzyldimethyltetradecylammonium chloride (BDTA), cetylpyridinium chloride and benzethonium chloride, all afford, under fast atom bombardment (FAB) mass spectrometric conditions, abundant and persistent [M---Cl]⁺ species usefully amenable to quantitative analysis with the aid of thioglycerol as a liquid FAB matrix. The use of BDTA as an internal standard allowed a direct, precise and accurate determination of cetylpyridinium and benzethonium chlorides, either as pure samples or in dosage forms, in the concentration range 0.05–2 mg/ml.     

天峨野生大果山楂酒中氨基酸与总黄酮的含量测定

目的：对天峨野生大果山楂（Malus doumeri)酒中氨基酸（游离氨基酸,水解氨基酸）,总黄酮进行含量测量。方法：利用高速氨基酸分析仪和分光光度计分别测定该酒中游离氨基酸,水解氨基酸和总黄酮类的含量。结果：该酒含17种游离氨基酸,含量为30．89％,16种水解氨基酸,含量为99．25％;总黄酮含量为15．43％（单位mg/ml)。结论：该酒富含氨基酸和总黄酮化合物,具有较强的生物活性。     

紫外光谱法测定利巴韦利葡萄糖注射液中利巴韦林的含量

目的建立利巴韦林葡萄糖注射液中利巴韦林的快速测定方法.方法用紫外分光光度法直接测定利巴韦林葡萄糖注射液中利巴韦林的含量.结果在207 nm处,以水为溶媒,利巴韦林葡萄糖注射液中利巴韦林浓度在3～15μg/ml,与其相应的吸收度呈良好的线性关系(n=5;r=0.999 9),样品平均回收率为101.4%±0.53%.结论该法简便快速、准确可靠,适合药房快速分析.     

基于UPLC对龙血通络胶囊特征图谱及5个成分含量的测定

目的 建立龙血通络胶囊超高效液相色谱法（UPLC）特征图谱,并测定7,4′-二羟基黄酮、4,4′-二羟基-2,6-二甲氧基二氢查耳酮、龙血素A、龙血素B、紫檀芪5个成分的含量。方法 采用Agilent Infinity Lab Poroshell 120 EC-C₁₈色谱柱（150 mm×3.0 mm,2.7 μm）,以乙腈（A）-0.1%磷酸水溶液（B）为流动相梯度洗脱,柱温为35 ℃,流速为0.5 mL·min^–1,进样体积为2 μL,检测波长为280 nm。结果 建立了龙血通络胶囊UPLC特征图谱,标定了13批样品中的11个共有特征峰,相似度均大于0.95。5个成分在相应质量浓度范围内呈良好的线性关系（r>0.999 5）,加样回收率为97.93%~107.33%,RSD均小于3.0%。结论 建立的UPLC操作简便、高效准确,可为龙血通络胶囊的质量控制提供参考。     

HPLC analysis of 16 compounds from Artemisia ordosica

Objective: To establish a high-performance liquid chromatographic method (HPLC) for the simultaneous determination of sixteen compounds from Artemisia ordosica. Methods: HPLC was used to analyze 16 quality indicators of A. ordosica. The HPLC conditions were as follows: Agilent Eclipse Plus C18 column (250 mm × 4.6 mm, 5 μm) with acetonitrile (A)-water (B) as mobile phase, gradient elution: 0?10 min, 75%?65% B; 10?30 min, 65%?35 % B; and finally 30?40 min, 35%?15% B. The flow rate was 1.0 mL/min, the column temperature was 40 °C, the injection volume was 10 μL, and monitored by absorbance at 285 nm for compounds 1?10, 12 and 225 nm for compounds 11, 13?16. Results: Under the selected experimental chromatographic conditions, compounds 1?16 showed good linearity (r > 0.9993) in a wide concentration range. Their average recoveries were 99.50%, 95.38%, 97.75%, 96.00%, 98.20%, 97.50%, 95.50%, 99.33%, 96.75%, 96.50%, 98.50%, 97.83%, 99.20%, 95.33%, 97.33% and 96.30%, respectively, and the RSD were 1.99%, 1.81%, 1.63%, 1.98%, 1.67%, 1.92%, 1.74%, 1.67%, 1.90%, 1.72%, 1.88%, 1.83%, 1.79%, 1.76%, 1.81% and 1.96%, respectively. Conclusion: Based on the results of the HPLC analysis, it was concluded that p-hydroxycinnamic acid (1), O-hydroxycinnamic acid (2), coniferyl alcohol (5), 5,4''-dihydroxy-7,3''-dimethoxyflavanone (8), 5,4''-dihydroxy-7-methoxyflavanone (9), 5-hydroxy-7,4''-dimethoxyflavanone (12), dehydrofalcarindiol (13), arteordoyn A (14), dehydrofalcarinol (15) and capillarin (16) are best suited for the role of quality indicators of A. ordosica grown in different ecological environments.     

基于指纹图谱和UPLC-MS/MS定量测定对不同产地陈皮的质量评价研究

目的 采用HPLC指纹图谱与化学计量学相结合、UPLC-MS/MS测定多黄酮成分含量的方法,测定不同产地陈皮质量,为其鉴别和质量控制提供依据。方法 采用HPLC-DAD指纹图谱检测并结合“中药色谱指纹图谱相似度评价系统（2012A版）”建立6个产区,49个不同批次陈皮药材（S1～S49）指纹图谱,并进行相似度评价和共有峰确认,结合聚类分析（hierarchical clustering analysis,HCA）、主成分分析（principal component analysis,PCA）、正交偏最小二乘法-判别分析（orthogonal partial least-squares discrimination analysis,OPLS-DA）等化学计量学综合分析。采用UPLC-MS/MS法建立了8个黄酮类成分柚皮素、柚皮苷、木犀草苷、川陈皮素、橙皮素、橙皮苷、橘皮素和芸香柚皮苷的含量测定方法对60批7个产地陈皮药材进行评价。结果 建立了49批不同产地陈皮药材的指纹图谱,相似度为0.864～0.999,共标定了11个共有峰,HCA分析49批陈皮明显分为4类;PCA得到5个主成分的累积方差贡献率为92.748%;OPLS-DA表明8、7、10和11号峰可能是影响陈皮药材质量的差异标志物;含量测定结果表明不同产地陈皮中黄酮类含量存在显著差异,广东新会以川陈皮素和橘皮素为主要标志成分,四川荷花池以木犀草苷为差异性成分,江西樟树以柚皮素和柚皮苷为差异性成分,广西玉林则以橙皮素、橙皮苷和芸香柚皮苷为主,重庆云阳以川陈皮素和橙皮苷为主。结论 建立了稳定性强的不同产地陈皮HPLC指纹图谱和8个黄酮类UPLC-MS/MS定量测定方法,结合化学计量学可用于陈皮药材综合评价和质量控制。     

中药配方颗粒辅料麦芽糊精的HPLC定量检测与中红外光谱半定量检测

目的 建立中药配方颗粒辅料麦芽糊精的检测方法,为中药配方颗粒质量评价提供分析技术支持。方法 建立配方颗粒中果糖、葡萄糖、蔗糖、麦芽糖、乳糖的HPLC定量检测方法,根据样品经糖化酶水解后的葡萄糖增加量换算出麦芽糊精含量。基于中药浸膏与麦芽糊精不同比例混合物的中红外光谱（mid-infrared spectroscopy,MIRS）特征峰差异,建立配方颗粒中麦芽糊精的半定量检测方法。结果 所建立的HPLC方法可以准确定量检测配方颗粒中果糖、葡萄糖、蔗糖、麦芽糖、乳糖。如果中药浸膏自身含有较多可经糖化酶水解产生葡萄糖的成分（淀粉、蔗糖等）,HPLC检测配方颗粒中麦芽糊精时存在系统性正误差,可通过中药浸膏酶解后葡萄糖增加量、待测样品酶解后蔗糖减小量等部分修正正误差。如果中药浸膏自身少含或不含淀粉、蔗糖等可经糖化酶水解产生葡萄糖的成分,HPLC检测配方颗粒中麦芽糊精时存在系统性负误差,换算公式偏差、麦芽糊精纯度、样品处理损失等导致根据样品酶解后葡萄糖增加量计算的麦芽糊精“检测含量”预期低于根据生产投料计算的麦芽糊精“名义含量”。麦芽糊精含量越高,配方颗粒MIRS中1200～900 cm-1区域的...     

Determination of diquat in biological materials by electron spin resonance spectroscopy

Summary An electron spin resonance (ESR) method already in use for the quantitative analysis of paraquat was applied to the analysis of diquat in blood, serum, urine, tissue homogenates and several drinks without purification of the samples. The diquat radical produced with ascorbic acid at alkaline pH was much more stable than that produced with the commonly used sodium dithionite. Radical decay in solutions covered with n-hexane was less than 5% after 60 min over a wide range of ascorbic acid concentrations. In 0.2N NaOH solution 85% of the radicals was present even after 24h. The limit of detection was 0.3 g/ml and the required amount of sample was 0.1 ml. When both diquat and paraquat were present in a sample the diquat was first extracted with 1-butanol prior to the ESR measurement, because both species were converted to the radicals.