高效体积排阻色谱-示差折光检测器-多角激光光散射仪联用测定右旋糖酐70原料药的分子质量

目的:建立测定右旋糖酐70原料药的分子质量的方法。方法:采用不需要对照品的高效体积排阻色谱-示差折光检测器-多角激光光散射仪(HPSEC-RID-MALLS)联用法,另与《中国药典》方法即HPSEC-RID法(采用3种来源对照品)测定3批样品重均分子质量(Mw)的结果进行比较。两种方法色谱柱均为TSK-GEL G4000SWXL凝胶色谱柱,流动相分别为0.2 mol/L氯化钠水溶液和0.71%硫酸钠水溶液(均含0.02%叠氮化钠)。结果:采用HPSEC-RID-MALLS法与采用其中2种来源对照品的HPSEC-RID方法测得的样品Mw结果相近。结论:HPSEC-RID-MALLS法不需要对照品,可直接测定样品的分子质量,方法更简便、快速,且结果准确。     

药用辅料检验用磷脂酰胆碱对照品的研制

目的：建立含量测定用的大豆磷脂酰胆碱、蛋黄磷脂酰胆碱对照品。方法：采用红外光谱、质谱、核磁对原料进行结构确证,卡氏水分测定法测定水分,采用ICP-MS测定金属离子含量,采用HPLCELSD标准曲线法测定纯度,以质量平衡法计算对照品含量。结果：红外光谱、质谱、核磁确证了大豆磷脂酰胆碱、蛋黄磷脂酰胆碱对照品的结构;大豆磷脂酰胆碱、蛋黄磷脂酰胆碱水分测定结果分别为2.2%,2.1%;大豆磷脂酰胆碱、蛋黄磷脂酰胆碱金属离子含量分别为0.03%,0.01%;纯度测定结果分别为99.3%,95.6%;通过质量平衡法计算各对照品含量分别为97.1%,93.6%。结论：建立了大豆磷脂酰胆碱和蛋黄磷脂酰胆碱对照品,可用作药用辅料磷脂含量测定用对照品。     

倍他米松磷酸钠标准改进及其对照品干燥失重方法修订的建议

目的:建立倍他米松磷酸钠标准中水分检测方法.方法:比较不同的干燥失重条件以及水分测定的结果,并通过动态水分吸附仪(DVS)对样品进行了考察.结果:采用水分测定法替代干燥失重检查可以避免干燥失重后样品降解.对照品使用前测定水分可以避免引湿性对对照品量值准确性的影响.结论:方法准确、方便,可作为倍他米松磷酸钠的水分检测方法.     

彝药水指甲药材的质量标准研究

目的:建立彝药水指甲药材的质量标准。方法:分别对水指甲药材进行性状鉴别和粉末显微鉴别,再以β-谷甾醇为对照品进行薄层色谱(TLC)鉴别;采用《中国药典》方法测定不同产地水指甲药材的水分、总灰分、酸不溶性灰分、醇溶性浸出物并制定其限度。结果:样品性状和显微鉴别特征明显,TLC特征斑点清晰,水分、总灰分、酸不溶性灰分、醇溶性浸出物的平均百分含量分别为9.5%、12.9%、2.6%、22.5%。结论:所建标准可用于水指甲药材的质量控制。     

人源化抗叶酸受体抗体的抗原结合活性测定

目的:采用直接ELISA法检测人源化抗叶酸受体抗体的抗原结合活性。方法:以固定量的重组人叶酸受体a做包被抗原,辣根过氧化酶标记的抗人IgG(H+L)为二抗,直接测定不同浓度参比品和供试品与抗原的结合活性,通过数据处理软件对结果绘图,根据供试品及参比品EC50值计算供试品的相对结合力。结果:同一批次的3支供试品分别经3次测定,相对结合活性分别为参比品的(80.61±12.19)%,(88.82±12.70)%,(103.57±6.07)%,平均值(91.0±13.72)%。3次试验的RSD分别为15.12%,14.30%,5.86%。结论:直接ELISA法精密性良好,结果客观,影响因素少,可用于人源化叶酸受体抗体抗原结合活性的常规检测。     

间接水解法测定含甲氧基黄酮UGT代谢物的摩尔消光系数转化因子

目的:建立测定含甲氧基黄酮尿苷二磷酸葡萄糖醛酸转移酶(UGT)代谢物转化为相应苷元的摩尔消光系数转化因子(K)的方法,实现对无对照品代谢物的准确定量。方法:以间接水解法测定含甲氧基黄酮汉黄芩素、杨芽黄素、泽兰黄素及5-羟基-7,8-二甲氧基黄酮的UGT代谢物K值;且因汉黄芩素及其UGT代谢物汉黄芩苷均有对照品,采用两对照品直接测定汉黄芩苷K值以验证间接水解法的准确性。结果:间接水解法测得上述含甲氧基黄酮UGT代谢物的K值分别为(1.05±0.03)、(1.47±0.09)、(1.04±0.04)、(1.25±0.09),直接测定汉黄芩苷的K值为(1.03±0.02),与间接法所测K值相近。结论:采用间接水解法测定K值可准确对无对照品黄酮化合物UGT代谢物进行定量。     

分光光度法测定甘草中总黄酮的含量

目的:建立分光光度法测定甘草中总黄酮含量。方法:利用二氢黄酮类在碱性条件下易转化为它的相应异构体-查尔酮类化合物特性,采用分光光度法,以甘草苷为对照品,以10%氢氧化钾为显色剂,在波长为400nm 处对样品中的总黄酮进行含量测定。结果:总黄酮在2.05-41.13μg·mL~(-1)范围内呈良好的线性关系(r=0.9992);该法的平均加样回收率分别为97.6%,RSD 分别为2.0%(n=3)。结论:该方法稳定、简便、快速,适用于甘草中总黄酮含量的测定。     

气相色谱法测定青翘挥发油中β-蒎烯的含量

目的:建立测定青翘挥发油中β-蒎烯含量的方法,并测定其含量。方法:采用无水乙醇纯化粗提取青翘挥发油;采用气相色谱法测定β-蒎烯含量。结果:用环己酮作为内标物;β-蒎烯对照品在0.3～4.4mg·mL~(-1)浓度范围内线性关系良好(r=0.9999);对照品和样品精密度的RSD分别为0.95%,0.99%(n=5);测得平均加样回收率为98.5%,RSD为1.2%(n=5);青翘挥发油中β-蒎烯含量为10.2%～10.2%,平均含量为10.2%,RSD为1.0%。结论:本方法快速准确可靠,简便易行,可用于青翘挥发油的质量控制。     

苯酚-硫酸法结合校正因子法测定含半乳糖醛酸的多糖中的糖含量

目的:建立一种基于苯酚-硫酸法结合校正因子法测定含半乳糖醛酸(GalA)的多糖中糖含量的方法。方法:优化苯酚-硫酸法的测定条件,以不同质量比的GalA-葡萄糖(Glc)混合对照品溶液绘制系列标准曲线并测定含GalA的党参多糖CPP1b样品中的糖含量,在此基础上,根据GalA-Glc质量比为0-100%时的回归方程,以党参多糖CPP1b为参照多糖计算校正因子,对样品中的糖含量测定结果进行校正,并以与党参多糖CPP1b组成相同的混合单糖对照品对此方法合理性进行验证。结果:经计算,党参多糖CPP1b对Glc的校正因子为3.33,验证试验中与党参多糖CPP1b组成相同的混合单糖对照品的糖含量测定结果为103.47%。精密度、稳定性试验的RSD<1%;加样回收率为93.52%~107.35%(RSD=5.09%,n=6)。结论:该研究建立的方法可准确测定类似于党参多糖CPP1b的含GalA的多糖中的糖含量。     

蓝萼香茶菜药材的质量标准研究

目的建立蓝萼香茶菜的质量标准。方法以咖啡酸为对照品,采用薄层色谱法对药材进行定性鉴别;采用高效液相色谱法对芦丁、齐墩果酸和熊果酸进行含量测定;并根据2015年版中国药典对蓝萼香茶菜药材的水分、总灰分、酸不溶性灰分进行定量测定。结果 TLC分离度良好,斑点清晰。芦丁、齐墩果酸及熊果酸分别在0.1838~2.7570 mg·mL~(-1)、0.009 98~0.149 70 mg·mL~(-1)及0.01132~0.169 80 mg·mL~(-1)与峰面积线性关系良好,含量分别不得少于0.2%、0.05%及0.08%。7批蓝萼香茶菜样品的水分测定结果为9.93%~10.81%,总灰分测定结果为8.17%~9.45%,酸不溶性灰分测定结果为2.87%~3.61%。结论上述方法简便,高效,专属性强,可有效控制蓝萼香茶菜药材的质量。     

How many pregnant women in Christchurch are using folic acid supplements in early pregnancy?

AIMS: To determine the proportion of pregnant women in Christchurch using folic acid supplements in early pregnancy. To evaluate the level of current knowledge relating to folic acid amongst pregnant women. To determine the main sources from which this information was gained. METHODS: A short questionnaire was administered to 191 pregnant women in Christchurch during antenatal visits with their lead maternity carer. The survey contained questions relating to knowledge about folic acid and use together with sources of information regarding folic acid. Obstetric and demographic details were also collected. RESULTS: The response rate was 95.5%. Ninety-one per cent (174/191) of participants had heard of folic acid and, of these, 63% knew that folic acid reduces the risk of spina bifida. Of the 191 participants in the study, 118(62%) took folic acid supplements at some stage of their pregnancy, however, only 33(17%) had taken periconceptual folic acid supplements. Of the 44% of all women in the study with a planned pregnancy, only 35% had taken folic acid supplements periconceptually. Of those women with an unplanned pregnancy (55%), only 2.8% had taken a folic acid supplement periconceptually. The main sources of advice for women relating to folic acid were general practitioners (48%) or media advertising, either in the form of a magazine, or health pamphlet or television promotion (20%). CONCLUSIONS: The results of this study indicate that the level of knowledge amongst women of child-bearing age relating to folic acid is relatively high compared with other countries. Despite this high level of knowledge, only a small percentage of women are actually consuming a folic acid supplement during the recommended periconceptual period due in part to the high proportion of unplanned pregnancies. These results emphasize the need for an effective public health strategy to ensure that all women of child-bearing age have access to an adequate folic acid intake.     

Maternal knowledge, attitude and practice on folic acid intake among Arabian Qatari women

BACKGROUND: Periconceptional folic acid supplementation is effective in preventing primary and secondary neural tube defects (NTDs) and other congenital defects. It is important to estimate folate intake and knowledge in women of child-bearing age, in relation to risk of congenital anomalies. AIM: The aim of this study was to determine the level of knowledge about the usefulness of periconceptional folic acid supplementation in a sample of women in the child-bearing age. DESIGN: This is a cross-sectional survey. SETTING: Eleven primary health care centers and women's hospital in Qatar. SUBJECTS: A multistage sampling design was used and a representative sample of 1,800 Qatari women aged between 18 and 45 years were surveyed during the period June to November 2004. One thousand four hundred and eighty women (82.2%) expressed their consent to participate in this study. METHODS: A confidential, anonymous questionnaire was completed by the selected subjects assessing folic acid awareness. Questionnaires were administered to women who were seeking routine antenatal care at health centers and Women's Hospital. Questions covered knowledge and use of folic acid supplements, pregnancy intention, and demographic and socioeconomic characteristics. Factors affecting study outcomes were examined individually by computing crude odd ratios and adjusted for other covariates using unconditional logistic regression. RESULTS: Out of 1480 women surveyed, 53.7% of them reported that they heard of folate. Of these, only half of the subjects knew that folate was something important. Overall, 20.3% of the respondents took folic acid. The most common information sources on folate were physicians (63.4%), and newspapers/magazine/books (21.7%). From those who heard of folate, only 14% knew that it can prevent birth defects. 40.6% of the subjects who heard folate were aware that green leafy vegetables were fortified with folic acid. In univariate analysis, awareness of folic acid was significantly associated with education of mother. Again, higher educated women (41.3%) knew more about folic acid and used it more often in the periconceptional and first trimester period. CONCLUSION: Awareness and use of folic acid was less prevalent among Qatari women. Educated women were aware of the importance of the intake of folic acid. The study findings suggested possible avenue for intervention to increase awareness and intake of folic acid.     

叶酸的光化学行为及其应用

目的：研究叶酸的光化学行为并提出测定叶酸的光化学荧光分析方法。方法：叶酸在六次甲基四胺-盐酸介质中,经365 nm紫外光照射后,发生光化学反应,产物的荧光强度(λ_ex 280 nm,λ_em 443 nm)较叶酸本身的增大了25倍。根据光化学反应产物的荧光强度测定叶酸的含量。结果：叶酸的浓度在1.0×10^-5～1.0×10^-7 mol.L^-1范围内,荧光强度与浓度呈良好的线性关系,检出限为1.5×10-9 mol.L^-1,相对标准偏差为1.6%。结论：本方法适用于片剂中叶酸的测定。     

替代对照品法测定龙血竭原料中龙血素A和B的含量

目的:建立替代对照品法同时测定龙血竭原料剑叶龙血树中龙血素A、B的含量。方法:提出了相对斜率的概念,解释了它与相对校正因子的数学关系,阐释了相对斜率(相对校正因子)的物理意义,进而采用相对斜率算法建立剑叶龙血树的含量测定法,并进行方法学验证。结果:方法的线性和回收率均良好;以龙血素A为参照,龙血素B的相对斜率和相对保留时间平均值为1.248和1.06,且在5个不同的色谱系统上保持稳定;相对斜率值与使用紫外分光光度计按吸光系数法测得值一致。结论:相对斜率算法简便、准确,以此进行替代对照品法测定剑叶龙血树中龙血素A、B是可行的。     

一测多评法测定冠心丹参颗粒中4种成分的含量

目的：建立以丹参酮Ⅱ_A内参物,同时测定冠心丹颗粒中丹参素钠、原儿茶醛、丹酚酸B、丹参酮Ⅱ_A的一测多评HPLC法。方法：以丹参酮Ⅱ_A为内参物,确定其他3种成分相对于丹参酮Ⅱ_A的校正因子,通过相对校正因子（RCF）对丹参素钠、原儿茶醛、丹酚酸B进行定量,实现一测多评（计算法）;同时采用外标法测定冠心丹参粒中4种成分的含量（实测法）,并比较一测多评法与外标法测定结果的差异。结果：在一定的线性范围内,丹参酮Ⅱ_A与丹参素钠、原儿茶醛、丹酚酸B的相对校正因子分别为0.299 9,1.991 7,0.424 4;且在不同实验条件下重复性良好（RSD分别为1.33%、1.44%、4.00%）;3批冠心丹参颗粒中4种成分按一测多评方法与外标法测定结果基本一致（RSD<3.0%）。结论：可有效地控制冠心丹参颗粒的内在质量。     

Awareness and use of folic acid, and blood folate concentrations among pregnant women in northern China--an area with a high prevalence of neural tube defects

BACKGROUND: The prevalence of neural tube defects (NTDs) in northern China remains high after 10 years since periconceptional supplementation with folic acid has been known to be effective in reducing the risk of NTDs. OBJECTIVE: The objectives of this study were to characterize folic acid awareness and use and to examine the association between folic acid supplementation with blood folate concentrations among early pregnant women in an area with a high prevalence of NTDs in northern China. SUBJECT AND METHOD: From December 2002 to February 2004, 693 early pregnant women were recruited and interviewed about folic acid awareness, knowledge and use. Four millilitres of venous blood was drawn and blood folate concentrations were measured. RESULTS: About 36% of women reported having ever heard of folic acid. Of these, 82.7% knew that folic acid can prevent NTDs, and 64.5% knew the best time to take it. Overall, 15% of women reported having ever taken folic acid. However, only 34.3% had begun to take it before the last menstrual period. Women with less education (21.1%), farmers (19.6%), rural dwellers (23.5%), and women who had a previous child (23.0%) were less likely to be aware of folic acid, and were less likely to take folic acid. Among women who had ever heard of folic acid, 37.5% took it during current pregnancy, compared with only 2.0% among those who had not. Women who were aware of folic acid were 25 times more likely to take it than women who were not. Overall, 44% of women had plasma folate deficiency, and 35% had red cell folate deficiency. Those who reported having ever taken folic acid had a lower rate of plasma folate deficiency (13.7%), compared with those who reported not taking folic acid (49.4%). The former group's mean plasma concentrations were twice as high as those of the latter group. CONCLUSION: The levels of folic acid awareness, knowledge and use among Chinese women living in a high NTD prevalence area during early pregnancy were very low and folate deficiency was quite prevalent. Campaigns aimed at increasing the awareness, knowledge, and periconceptional use of folic acid should target to less educated, parous women and women living in rural areas.     

Influence of green and black tea on folic acid pharmacokinetics in healthy volunteers: potential risk of diminished folic acid bioavailability

Previous in vitro studies using Caco-2 cell monolayers suggested a possible interaction between green and black tea and folic acid at the level of intestinal absorption. The main purpose of the present study was to investigate a possible pharmacokinetic interaction between tea and folic acid in healthy volunteers. In an open-labeled randomized cross-over study, the pharmacokinetic interaction between tea and folic acid (0.4 mg and 5 mg) was investigated in healthy volunteers. Water was used as the reference drink. Subjects ingested 0.4 mg folic acid tablets with water, green or black tea (0.3 g extract/250 ml) or 5 mg folic acid tablets with water or green tea (0.3 g extract/250 ml). Blood samples were collected over a period of 8 h. Serum folate analysis was carried out by a competitive immunoassay which uses direct chemiluminescent technology. At the 0.4 mg folic acid dose, green and black tea reduced the mean C(max) of serum folate by 39.2% and 38.6%, and the mean AUC(0 --> infinity) by 26.6% and 17.9%, respectively. At the 5 mg folic acid dose, the mean C(max) of serum folate was reduced by 27.4% and the mean AUC(0 --> infinity) was decreased significantly by 39.9% by the co-application of green tea. The present results suggest an in vivo interaction between tea and folic acid with even low concentrations of green and black tea extracts yielding decreased bioavailabilities of folic acid. Copyright (c) 2008 John Wiley & Sons, Ltd.     

唐山地区3家医院脑梗死二级预防中叶酸的应用现况调查

目的:了解唐山市部分医院脑梗死二级预防中叶酸的应用现状,找到与相关指南之间的差距,为改进脑梗死二级预防工作提供参考。方法:研究对象为唐山市3家医院诊断为脑梗死的住院患者共573例,按照血浆总同型半胱氨酸(tHcy)水平将入选病例分为3组,调查不同组别患者二级预防中叶酸的应用现状。结果:叶酸的使用率在血浆tHcy重度升高组为62.9%,在中度升高组中为50.7%,在轻度升高组中为38.1%,3组间比较差异有统计学意义(P<0.05);但叶酸的使用量3组间比较差异无统计学意义(P>0.05)。结论:唐山地区部分医院对叶酸应用于脑梗死二级预防已经有了一定程度的认识,但使用率、使用量等与相关指南尚有距离,需进一步加强对医务人员的培训。     

Bioavailability of oral vs. subcutaneous low-dose methotrexate in patients with Crohn's disease

BACKGROUND: Oral methotrexate and folic acid are partly absorbed by a common intestinal transporter. AIM: : To determine the relative bioavailability of oral low-dose methotrexate administered with and without concomitant folic acid vs. subcutaneous administration in patients with stable Crohn's disease. METHODS: Ten patients were randomized to receive their regular maintenance dose of methotrexate (15-25 mg) for three consecutive weeks: orally, orally with 5 mg folic acid or subcutaneously. Blood samples were drawn at specified intervals during 24 h, and methotrexate levels were determined by fluorescence immunoassay. Areas under the curve extrapolated to infinity (AUC infinity ) were compared between the three routes. RESULTS: The geometric mean AUC infinity values (95% confidence intervals) were 360 nmol x h/L (301-430 nmol x h/L), 261 nmol x h/L (214-318 nmol x h/L) and 281 nmol x h/L (209-377 nmol x h/L) per milligram of methotrexate administered for subcutaneous, oral and oral with folic acid administration, respectively (P < 0.05 and P < 0.01 for oral with folic acid and oral vs. subcutaneous administration, respectively). The geometric mean relative bioavailabilities (95% confidence intervals) were 0.73 (0.62-0.86) and 0.77 (0.60-0.99) for oral and oral with folic acid administration, respectively (difference not significant). CONCLUSIONS: In patients with stable Crohn's disease, the oral bioavailability of methotrexate is highly variable and averages 73% of that of subcutaneous administration. Concomitant folic acid has no significant effect on the bioavailability. Dose adjustments based on individual pharmacokinetic assessment should be considered when switching patients from parenteral to oral therapy.