HPLC测定早产儿咖啡因血药浓度

目的 建立HPLC测定早产儿咖啡因血药浓度的方法。方法 色谱柱为Insertil ODS-3（250 mm×4.6 mm,5 μm）,甲醇-水（28：72）为流动相,流速1 mL·min^-1,检测波长274 nm,柱温30℃,进样量20 μL。结果 咖啡因血药浓度在2.5~60 mg·L^-1内呈良好的线性关系（r²=0.999 9,n=9）,定量限为0.125 mg·L^-1。提取回收率为82.5%~89.7%,方法回收率为97.2%~103.0%;日内与日间精密度RSD均<10%。随机检测5名负荷剂量给药的患儿次日咖啡因谷浓度为（15.8±2.1） mg·L^-1,另5例患儿给药7 d后检测咖啡因谷浓度为（24.3±4.6） mg·L^-1,均在有效线性范围内。结论 本方法灵敏、可靠,可作为咖啡因血药浓度的常规监测方法。     

UPLC-MS/MS测定减肥食品中8种非法添加化学成分

目的 建立一种简便有效检测减肥食品中非法添加化学成分的UPLC-MS/MS检测方法。方法 采用UPLC-MS/MS法,以Eclipse Plus C₁₈（2.1 mm×50 mm,1.8 μm）色谱柱分离,串联四级杆质谱仪检测,多反应监测模式进行定性定量分析,以流动相A（0.02 mol·L^-1乙酸铵水溶液）-B（甲醇）进行梯度洗脱;柱温：40℃;流速：0.3 mL·min^-1,进样量2 μL。样品以甲醇为溶剂超声提取,快速定性定量检测非法添加在减肥食品中的麻黄碱、咖啡因、呋塞米、芬氟拉明、酚酞、N-单去甲基西布曲明、N,N-双去甲基西布曲明、西布曲明8种化学成分。结果 8种减肥类化学成分质谱检测的线性范围宽,相关性R² ≥ 0.995;方法检测限为0.042~0.175 μg·mL^-1,定量限为0.126~0.525 μg·mL^-1,方法精密度RSD（n=6）为1.7%~4.7%;3个浓度水平的平均回收率为90.3%~105.1%。结论 本方法专属性强、操作简单、方便快捷,可作为食品中非法添加减肥类化学成分的有效检测方法。     

菟丝草质量标准研究

目的：建立菟丝草质量标准。方法：采用TLC法鉴别;采用HPLC法测定菟丝草中金丝桃苷的含量,色谱柱为Agilent Eclipse TC-C18 （250 mm×4.6 mm,5 μm）,流动相为乙腈-0.1%磷酸溶液（17∶83）,流速为1.0 mL·min^-1,柱温为30 ℃,检测波长360 nm。 结果：TLC色谱斑点清晰,金丝桃苷在2.568~206.4 μg·mL^-1范围内线性关系良好（r=0.9999）,平均回收率为100.18%,RSD为2.09% （n=9） 。结论：本方法准确、简便、灵敏度高,能有效控制菟丝草药材的质量。     

HPLC-ELSD和IC-ICD检测磺丁基-β-环糊精中的杂质离子

目的 建立了高效液相色谱-蒸发光散射法（HPLC-ELSD）及离子色谱-抑制电导检测法（IC-ICD）测定磺丁基-β-环糊精中氯化钠、4-羟基-1-丁烷磺酸钠、双（4-磺丁基）醚二钠3种杂质含量的方法。方法 HPLC-ELSD采用CD-Screen-IEC柱（4 mm×150 mm，3 μm），梯度洗脱，流速为1.2 mL·min^-1；IC-ICD采用Dionex IonPac AS19（4 mm×250 mm）阴离子交换色谱柱分离，30 mmol·L^-1氢氧化钠溶液为淋洗液，等度洗脱，流速为1.0 mL·min^-1。结果 2种方法各组分分离度良好，HPLC-ELSD法中氯化钠、4-羟基-1-丁烷磺酸钠、双（4-磺丁基）醚二钠检出限（S/N=3）分别为0.230，0.270和0.340 ng，IC-ICD法检出限分别为0.041，0.027和0.014 ng。结论 HPLC-ELSD和IC-ICD在磺丁基-β-环糊精中氯化钠、4-羟基-1-丁烷磺酸钠、双（4-磺丁基）醚二钠3种杂质的含量测定结果上没有明显不同，可根据实际情况选择，只是根据2种方法的检出限及定量限值，IC-ICD法灵敏度更高。     

藏药石榴莲花散中鞣花酸和胡椒碱含量测定方法研究

目的： 建立藏药石榴莲花散中鞣花酸和胡椒碱含量测定方法,以完善其质量标准。方法： 采用高效液相色谱法测定制剂中石榴子和诃子的鞣花酸含量,采用ODS-2 HYPERSIL C₁₈色谱柱（4.6 mm×250mm,5 μm）,以乙腈-0.2%磷酸（15：85）为流动相,流速1.0 mL·min^-1,检测波长254 nm,柱温30℃;采用高效液相色谱法测定制剂中荜茇的胡椒碱含量,采用ODS-2 HYPERSIL C₁₈色谱柱（4.6mm×250 mm,5μm）,以乙腈-水（40：60）为流动相,流速1.0 mL·min^-1,检测波长343 nm,柱温30℃。结果： 鞣花酸进样量在5.065~25.325 μg范围内呈良好线性关系（r=0.9999）,平均回收率为97.5%,RSD=1.5%（n=6）;胡椒碱进样量在10.414~52.071 μg范围内呈良好线性关系（r=1.0000）,平均回收率为99.6%,RSD=0.6%（n=6）。结论： 该方法可准确测定石榴莲花散中鞣花酸和胡椒碱的含量,有助于提高石榴莲花散的质量标准。     

GC同时测定藏药七味铁屑丸中4种物质的含量

目的 建立同时测定藏药七味铁屑丸中土木香内酯、异土木香内酯、去氢木香内酯和木香烃内酯的GC法。方法 HP-5毛细管色谱柱（30 m×0.32 mm,0.25 μm）;FID检测器;柱温箱温度140℃,进样口温度220℃,检测器温度250℃;载气为氮气,流速为1.0 mL·min^-1,空气流速450 mL·min^-1,氢气流速45 mL·min^-1;进样量1 μL;分流比20︰1。结果 土木香内酯、异土木香内酯、去氢木香内酯和木香烃内酯的线性范围分别为7.120 2~71.202 2 μg·mL^-1（r=0.998 4）;5.478 5~54.785 1 μg·mL^-1（r=0.997 1）;8.195 3~98.344 1 μg·mL^-1（r=0.996 7）;6.395 4~76.744 8 μg·mL^-1（r=0.997 2）;平均回收率分别为98.11%（RSD=1.04%）,98.12%（RSD=1.09%）,98.39%（RSD=1.26%）,97.52%（RSD=1.25%）。结论 本方法可有效可靠地对七味铁屑丸中藏木香和木香进行定量控制。     

藏药七味诃子散中有效成分丁香酚的含量测定

目的：建立七味诃子散中丁香酚含量的HPLC测定方法。方法：采用Phenomenex Luna 5 μ C18色谱柱（4.6 mm×250 mm,5 μm）,流动相为甲醇-水（55：45）,流速为1 mL·min^-1,检测波长为柱温为25℃。结果：丁香酚的进样量在0.564~2.820 μg范围内线性关系良好（r=0.9999）,平均回收率为99.03%（RSD=1.01%）;样品中丁香酚的含量测定结果为14.7~15.6 mg·g^-1。结论：本方法可用于测定七味诃子散中丁香酚的含量,可为该药质量标准修定提供参考。     

HPLC法同时测定宫颈炎康栓中苦参碱和槐定碱的含量

目的：建立宫颈炎康栓中苦参碱和槐定碱的HPLC测定方法。方法：采用Ultimate XB-NH2色谱柱（4.6 mm×250 mm，5 μm），流动相为乙腈-3%磷酸溶液（97︰3），流速为1.0 mL·min^-1，检测波长206 nm，柱温35℃。结果：苦参碱进样量在0.05095~2.5475 μg范围内线性关系良好（r=1.0000），平均回收率为98.0%；槐定碱进样量在0.05144~2.5720 μg范围内线性关系良好（r=1.0000），平均回收率为99.9%。结论：本法经方法学验证，可用于中成药宫颈炎康栓的质量控制。     

HPLC测定四味珍层冰硼滴眼液中苯氧乙醇含量

目的 采用HPLC测定四味珍层冰硼滴眼液中苯氧乙醇含量。方法 采用DIKMA Diamonsil C₁₈色谱柱（4.6 mm×250 mm,5 μm）;流动相：甲醇-水（50∶50）;流速： 1.0 mL·min^-1;检测波长： 268 nm;柱温： 30℃。结果 苯氧乙醇在浓度5.43~163.04 μg·mL^-1内线性关系良好（r=1.000 0）,平均回收率为100.3%,RSD为1.1%。结论 该法简便、准确、精密度高,适用于四味珍层冰硼滴眼液中苯氧乙醇含量测定。     

HPLC法测定蒙药巴日嘎-13散中大叶茜草素的含量

目的：建立高效液相色谱法测定巴日嘎-13散中茜草有效成分大叶茜草素的含量。方法：DikmaDimonsil C18色谱柱（250 mm×4.6 mm,5 μm）,流动相为甲醇-水-四氢呋喃（527：90：3）,检测波长为391nm,流速为1 mL·min^-1。结果：大叶茜草素在5.5~55 μg·mL^-1范围内呈良好的线性关系（r=0.9999）,平均加样回收率为102.24%,RSD为1.48%。结论：本方法简便可靠、分离度较好、结果稳定,可用于巴日嘎-13散的质量检测。     

鼻渊净胶囊的HPLC指纹图谱研究

目的 建立鼻渊净胶囊的高效液相色谱(HPLC)指纹图谱.方法 采用Agilent SB-C18(4.6 mm×250 mm,5μm)色谱柱,乙腈-水为流动相、以1.0 ml/min流速行梯度洗脱,检测波长210 nm,柱温30℃,洗脱时间为80 min.采用中药色谱指纹图谱相似度评价系统(2004A版)对检测出色谱进行...     

Synthesis and evaluation of 2,6-piperidinedione derivatives as potentially novel compounds with analgesic and other CNS activities

New 2,6-piperidinediones 2_a–g and 4_a–d were prepared by initial condensation of aromatic aldehydes or cycloalkanones with cyanoacetamide to give α-cyanocinnamides l_a–g or cycloalkylidenes 3_a,b which underwent Michae1 addition with ethyl cyanoacetate or diethylmalonate. Compounds 4_a–d were alkylated by various alkyl halides to produce the N-alkylated 2,6-piperidinedione derivatives 5_a–m. Some new selected compounds 2_a–c,f, 4_a–d & 5_e,h,j were pharmacologically evaluated for potential anticonvulsant, sedative and analgesic activities. These compounds exhibited significant anticonvulsant and analgesic effects after a single I.P. administration 100 mg/kg b.wt. . On the other hand all the investigated compounds induced hypnotic activity and prolonged the phenobarbital sodium- induced sleep as compared with the control group and the most potent compound was found to be 2_f.     

Investigation of the prevalence of tetQ, tetX and tetX1 genes in Bacteroides strains with elevated tigecycline minimum inhibitory concentrations

In this study, the antibiotic susceptibilities to tigecycline and tetracycline of 35 selected Bacteroides fragilis group strains were determined by Etest, and the presence of tetQ, tetX, tetX1 and ermF genes was investigated by polymerase chain reaction (PCR). tetQ was detected in all 12 B. fragilis group isolates (100%) exhibiting elevated tigecycline minimum inhibitory concentrations (MICs) (≥8 μg/mL) as well as the 8 strains (100%) with a tigecycline MIC of 4 μg/mL, whilst tetX and tetX1 were present in 15% and 75% of these strains, respectively. All of these strains were fully resistant to tetracycline (MIC ≥ 16 μg/mL). On the other hand, amongst the group of strains with tigecycline MICs < 4 μg/mL (15 isolates), tetQ, tetX and tetX1 were found less frequently (73.3%, 13.3% and 46.7%, respectively). All but two strains harbouring the tetQ gene in this group were non-susceptible to tetracycline, with a MIC > 4 μg/mL. These data suggest that in most cases tigecycline overcomes the tetracycline resistance mechanisms frequently observed in Bacteroides strains. However, the presence of tetX and tetX1 genes in some of the strains exhibiting elevated MICs for tigecycline draws attention to the possible development and spread of resistance to this antibiotic agent amongst Bacteroides strains. The common occurrence of ermF, tetX, tetX1 and tetQ genes together predicted the presence of the CTnDOT-like Bacteroides conjugative transposon in this collection of Bacteroides strains.     

抗幽门螺杆菌活性挥发油的筛选、药效物质分析及其作用机制预测

目的 探讨抗幽门螺杆菌（HP）活性挥发油的药效物质,初步预测潜在活性成分及其作用机制。方法 微量稀释法（96 微孔板）测定丁香、广藿香、紫苏、牛至、枳实、厚朴、薄荷、肉桂 8 种挥发油对 HP 的抑制率,筛选出抑菌活性最强的 3种挥发油。气相色谱-质谱法联用（GC-MS）分析 3 种挥发油的化学成分,利用 TCMSP、Swiss Target Prediction、PubChem数据库获取 3 种挥发油主要活性成分及其对应靶点信息;网络药理学技术预测其潜在活性成分、相关通路及关键靶点;AUTO DOCK Vina 软件对核心成分及关键靶点基因进行分子对接,初步验证潜在活性成分及关键靶点。结果 广藿香、牛至和肉桂挥发油抑制 90% 细菌生长的最低药物浓度（MIC₉₀）分别为 0.250、0.250、0.125 μL·mL^-1,具有较强的抑菌活性;从以上 3 种挥发油中分别鉴定出 27、26、15 个化学成分,共筛选出 15 个活性成分,涉及 232 个基因靶点,影响了与抑制 HP相关的癌症通路、化学致癌-受体激活及 EGFR 酪氨酸激酶抑制剂耐药性等 275 条信号通路;分子对接验证结果显示 3 种挥发油抗 HP 与 SRC 蛋白密切相关,15 个活性成分与关键靶点 SRC 的结合较为稳定。结论 广藿香、牛至、肉桂 3 种活性挥发油通过多成分、多靶点、多通路的形式发挥抗 HP 作用。     

栝楼不同药用部位质量控制的研究进展

瓜蒌子、瓜蒌皮、瓜蒌、天花粉来源于栝楼的不同药用部位,4味药材均为常用的大宗药材,现行版《中国药典》对其制定的质量标准过于简单,无法科学合理地控制其质量。本文对瓜蒌子、瓜蒌皮、瓜蒌、天花粉安全性和有效组分的研究进行综述,明确了相关研究存在的问题并针对问题提出建议,为科学全面的药材及饮片标准的制定提供参考依据。     

喙果黑面神化学成分研究

目的研究大戟科植物喙果黑面神(Breynia rostrata Merr.)的化学成分。方法利用硅胶、凝胶等色谱技术分离纯化化学成分,根据化合物的理化性质和光谱数据进行结构鉴定。结果从喙果黑面神的正丁醇萃取部分分离得到4个化合物,分别鉴定为6-O-甲基丙酰基-α-D-吡喃葡糖(6-O-methylpropanoyl-α-D-glucopyranose,1);4″-苯酚基-6-O-甲基丙酰基-β-D-吡喃葡糖苷(4″-phenolic-6-O-methylpropanoyl-β-D-glucopyranoside,2);1-O-没食子酰基-β-D-吡喃葡糖苷(1-O-galloyl-β-D-glucopyranoside,3);熊果苷(arbutin,4)。结论化合物1和2为新化合物,3和4均为首次从该种植物分离得到。     

Reassessment of the toxin profile of Cylindrospermopsis raciborskii T3 and function of putative sulfotransferases in synthesis of sulfated and sulfonated PSP toxins

The toxigenic freshwater cyanobacterium Cylindrospermopsis raciborskii T3 has been used as a model to study and elucidate the biosynthetic pathway of tetrahydropurine neurotoxins associated with paralytic shellfish poisoning (PSP). There are nevertheless several inconsistencies and contradictions in the toxin profile of this strain as published by different research groups, and claimed to include carbamoyl (STX, NEO, GTX2/3), decarbamoyl (dcSTX), and N-sulfocarbamoyl (C1/2, B1) derivatives. Our analysis of the complete genome of another PSP toxin-producing cyanobacterium, Raphidiopsis brookii D9, which is closely related to C. raciborskii T3, resolved many issues regarding the correlation between biosynthetic pathways, corresponding genes and the T3 toxin profile. The putative sxt gene cluster in R. brookii D9 has a high synteny with the T3 sxt cluster, with 100% nucleotide identity among the shared genes. We also compared the PSP toxin profile of the strains by liquid chromatography coupled to mass spectrometry (LC-MS/MS). In contrast to published reports, our reassessment of the PSP toxin profile of T3 confirmed production of only STX, NEO and dcNEO. We gained significant insights via correlation between specific sxt genes and their role in PSP toxin synthesis in both D9 and T3 strains. In particular, analysis of sulfotransferase functions for SxtN (N-sulfotransferase) and SxtSUL (O-sulfotransferase) enzymes allowed us to propose an extension of the PSP toxin biosynthetic pathway from STX to the production of the derivatives GTX2/3, C1/2 and B1. This is a significantly revised view of the genetic mechanisms underlying synthesis of sulfated and sulfonated STX analogues in toxigenic cyanobacteria.     

银杏叶提取物与刺梨配伍抗实验性肝损伤作用

目的：比较复方银杏叶胶囊（CGB）与单方银杏叶提取物（GBE）的保肝作用。方法：用CGB、GBE给小鼠灌胃30d后,腹腔注射CCl4诱发肝损伤,测定小鼠血清丙氨酸氨基转移酶（ALT）、天门冬氨酸氨基转移酶（AST）及肝匀浆超氧化物歧化酶（SOD）、丙二醛（MDA）含量;用H2O2诱导人肝L-02细胞氧化损伤,观察细胞增殖及总抗氧化能力。结果：CGB2．4、0．8和0．4g／kg3个剂量组与模型组比较,小鼠血清ALT、AST明显降低（P〈0．01,P〈0．05）,同时肝匀浆中SOD显著升高、MDA下降（P〈0．01,P〈0．05）;CGB组细胞增殖率和总抗氧化能力分别较模型组和单方组显著提高（P〈0．05、P〈0．01）。结论：CGB的抗肝损伤作用优于单方银杏叶提取物。     

Chemopreventive effect of celecoxib in gastric cancer

COX (cyclooxygenase) is one of the key enzymes involved in the synthesis of a variety of prostaglandins (PGs), some of which have been strongly linked to inflammation. One of its two well-known isoforms, COX-2, is an inducible enzyme whose induction and expression is dynamically regulated by growth factors, mitogens, and tumor promoters. Several animal and clinical studies have reported the chemopreventive effect of celecoxib, a selective COX-2 inhibitor; and in particular, a few studies have shown that celecoxib prevents the development of gastric cancer. Administration of celecoxib also showed increases in cardiovascular risk and disruption of renal physiology. Therefore, studies hoping to clarify how selective COX-2 inhibitors modulate gastric cancer must keep in mind that coxibs have also been linked to serious cardiovascular events and disruption of renal physiology. Received 12 July 2006; accepted 21 August 2006     

2017—2020年克拉玛依市中心医院抗菌药物使用强度与分离菌耐药性变化情况

目的 分析克拉玛依市中心医院2017—2020年住院患者常见分离菌分布及耐药率的变迁情况,为指导抗菌药物临床合理应用提供依据。方法 收集2017—2020年克拉玛依市中心医院住院患者抗菌药物使用情况及分离菌,分析主要分离菌对常见抗菌药物的耐药率变化趋势。结果 2017—2019克拉玛依市中心医院抗菌药物使用率和使用强度呈下降趋势,4年共有分离菌12 135株,其中革兰阳性菌2 567株,占21.15%;革兰阴性菌6 310株,占52.00%;真菌3 258株,占26.85%。居前5位的分离菌分别是白色假丝酵母菌（19.59%）、大肠埃希菌（16.84%）、肺炎克雷伯菌（13.33%）、鲍曼不动杆菌（8.71%）和铜绿假单胞菌（7.94%）。主要分离菌对常用抗菌药物耐药率总体呈下降趋势,肠杆菌科细菌对临床常用抗菌药物耐药性下降最明显。结论 克拉玛依市中心医院分离菌逐年增加,耐药率有下降趋势,抗菌药物临床应用基本合理,但需完善真菌检测能力。