HPLC法同时测定泻肝安神丸中龙胆苦苷、栀子苷、黄芩苷的含量

摘 要 目的：建立HPLC法同时测定泻肝安神丸中龙胆苦苷、栀子苷、黄芩苷的含量。方法: 采用Phenomenex Luna C18(2)柱（250 mm×4.60 mm,5 μm）,以甲醇－0.2%磷酸溶液为流动相,梯度洗脱,流速为1.0 ml·min^-1,柱温为30℃,检测波长为254 nm,进样量为10 μl。结果: 龙胆苦苷在10.55~168.80 μg·mL^-1范围内线性关系良好（r=0.999 9）,平均回收率为98.68％,RSD为1.2％（n=6）;栀子苷在29.85~477.60 μg·mL^-1范围内线性关系良好（r=0.999 8）,平均回收率为98.76％,RSD为1.1％（n=6）;黄芩苷在43.05~688.80 μg·mL^-1范围内线性关系良好（r=0.999 7）,平均回收率为98.36％,RSD为1.4％（n=6）。结论:该方法简单、准确,可同时测定3种成分的含量,可用于泻肝安神丸的质量控制。     

HPLC法测定米诺地尔洗剂含量及温度对含量影响的考察

摘 要 目的：建立高效液相色谱法同时测定化瘀祛斑胶囊中芍药苷、黄芩苷和黄芩素的含量。方法: 色谱柱为Agilent Zorbax SB C18柱（150 mm×4.6 mm,5 μm）;流动相为甲醇 0.1%磷酸溶液,梯度洗脱;流速为1.0 ml·min-1;检测波长为230 nm（0~15 min）,277 nm（15~45 min）;柱温为25℃;进样量为10 μl。结果: 芍药苷、黄芩苷和黄芩素的线性范围分别为1.295～25.890 μg·ml-1（r=0.999 9）、30.050～601.000 μg·ml-1（r=0.999 9）、1.874~37.480 μg·ml-1（r=0.999 9）,平均回收率分别为100.9%,100.3%,99.31%,RSD分别为0.92%,1.30%,0.89%。结论: 该法简便、快捷、结果准确、重复性好、实用性强,可以用于化瘀祛斑胶囊的质量控制。     

HPLC法同时测定和肝利胆颗粒中栀子苷和黄芩苷的含量

摘 要 目的： 建立和肝利胆颗粒中栀子苷和黄芩苷的含量测定方法。方法: 采用高效液相色谱法,用Dionex C₁₈（250 mm×4.6 mm,5 μm）色谱柱,以甲醇为流动相A,0.5%冰醋酸溶液为流动相B,梯度洗脱,流速为1.0 ml·min^-1,检测波长为239 nm,柱温:30℃,进样量：10 μl。结果: 栀子苷和黄芩苷与其相邻杂质峰能完全分离,栀子苷在7.890～78.900 μg·mL^-1的浓度范围内有良好的线性关系,r=0.999 9;黄芩苷在8.020～80.200 μg·mL^-1的浓度范围内有良好的线性关系,r=0.999 9。栀子苷和黄芩苷的平均回收率分别为99.8%(RSD=2.1% ,n=6）和99.5%(RSD=1.5%,n=6）。结论: 本方法简便、准确、重复性好,可用于该药的质量控制的评价。     

HPLC法同时测定柔肝顺气丸中7种成分的含量

摘 要 目的：建立HPLC法同时测定柔肝顺气丸中氧化芍药苷、芍药内酯苷、芍药苷、丹参素、丹酚酸B、丹参酮ⅡA和α-香附酮的含量。 方法: 采用Agilent Eclipse XDB C18色谱柱（250 mm×4.6 mm,5 μm）,流动相为乙腈 0.1%甲酸溶液,梯度洗脱,检测波长分别为230,280,242 nm,流速为1.0 ml·min-1,柱温为30 ℃。 结果: 7种成分,氧化芍药苷、芍药内酯苷、芍药苷、丹参素、丹酚酸B、丹参酮ⅡA和α-香附酮分别在0.99～19.80,4.67～93.40,7.03～140.60,1.36～27.20,10.69～213.80,1.77～35.40,1.09～21.80 μg·ml-1范围内线性关系良好(r>0.999 0);平均加样回收率分别为97.12%,99.10%,100.01%,98.51%,100.04%,98.69%,97.88%,RSD分别为1.54%,0.86%,0.47%,1.28%,0.66%,1.04%,1.20%(n=9)。 结论: 该方法操作便捷、重复性好,可更加快速全面地对柔肝顺气丸进行质量分析和质量控制。     

双波长HPLC法同时测定复方肤清洗剂中3种指标性成分含量

摘 要 目的：建立双波长HPLC法同时测定复方肤清洗剂中绿原酸、咖啡酸、芍药苷3种指标性成分含量的方法。方法: 采用Inertsil C18柱（250 mm×4.6 mm,5 μm）为色谱柱,柱温40℃,以乙腈-0.02%磷酸水溶液（17∶83）为流动相,流速为1.0 ml·min^-1,检测波长分别为323 nm、230 nm。结果:绿原酸、咖啡酸和芍药苷分别在7.50~120.00 μg·mL^-1,2.50~40.00 μg·mL^-1,14.06~225.00 μg·mL^-1范围内线性关系良好,r分别为0.999 9,0.999 8,0.999 7;平均加样回收率分别为98.55%,94.52%,99.18%,RSD分别为1.66%,0.98%,0.65%（n=6）。结论:该方法简便快捷、结果准确、专属性强,可用于复方肤清洗剂的质量分析与控制。     

HPLC法同时测定肾炎四味胶囊中4种黄酮类成分的含量

摘 要 目的： 建立HPLC法同时测定肾炎四味胶囊中黄芩苷、黄芩素、汉黄芩苷、汉黄芩素等4种成分。方法: 采用Agilent ZORBAX SB-C₁₈（250 mm×4.6 mm,5 μm）色谱柱,流动相为甲醇 0.4%磷酸溶液,梯度洗脱,流速为1.0 ml·min^-1,检测波长为278 nm,柱温为30℃,进样量为10 μl。结果: 上述色谱条件下,4种成分分离较好,黄芩苷、黄芩素、汉黄芩苷和汉黄芩素线性关系良好,线性范围分别为0.060～1.203 μgr=0.999 9、0.026～0.521 μgr=0.999 9、0.031～0.622 μg（r=0.999 8）、0.025～0.497 μg（r=0.999 6）,加样回收率分别为97.9%（RSD=1.72%）、101.8%（RSD=1.86%）、102.1%（RSD=1.35%）、99.3%（RSD=1.12%）（n=9）。结论: 本方法准确度高、重复性好,能同时测定肾炎四味胶囊中黄芩苷、黄芩素、汉黄芩苷、汉黄芩素等4种成分的含量。     

多波长HPLC法同时测定皮肤康洗液中5种有效成分的含量

摘 要 目的：建立多波长切换高效液相色谱法同时测定皮肤康洗液中芍药苷、甘草苷、甘草酸铵、大黄素和蛇床子素5种有效成分的含量。方法: 色谱柱为 Diamonsil C18柱(200 mm×4.6 mm,5 μm);流动相为乙腈 0.1%盐酸水溶液,梯度洗脱;流速为1.5 ml·min^-1;柱温为30℃;检测波长为232 nm(0～6 min,检测芍药苷)、277 nm(6～10 min,检测甘草苷)、254 nm(10 min以后,检测甘草酸铵、大黄素、蛇床子素）。结果: 芍药苷、甘草苷、甘草酸铵、大黄素和蛇床子素的线性范围分别为28.20～282.0 μg·ml^-1（r=0.999 7）、12.150～121.500 μg·ml^-1（r=0.998 8）、13.420～134.200 μg·ml^-1（r=0.999 5）、0.047～0.466 μg·ml^-1（r=0.999 9）、2.380～23.800 μg·ml^-1（r=0.999 9）,平均加样回收率分别为98.49%,99.00%,98.38%,97.36%,97.70%,RSD分别为0.71%,0.62%,0.85%,0.92%,0.78%（n=6）。结论:该方法简便、准确、灵敏度高、重复性好,可用于同时测定皮肤康洗液中上述5个有效成分的含量。     

HPLC法测定黄连上清片中4种成分的含量

摘 要 目的： 提高黄连上清片质量标准,建立同时测定绿原酸、栀子苷、黄芩苷、盐酸小檗碱4种成分含量的方法。方法: 采用高效液相色谱法,色谱柱为DiamonsilTM C₁₈(250 mm×4.6 mm,5 μm),流动相为二元梯度系统,其中溶剂A为乙腈,溶剂B为0.3%磷酸水溶液,流速为1.0 ml·min^-1,检测波长为238 nm,柱温30℃,进样量为10 μl。结果: 绿原酸、栀子苷、黄芩苷、盐酸小檗碱的线性范围分别为8.11～81.10 μg·ml^-1(r=0.999 7)、13.08～130.80 μg·ml^-1(r=0.999 7)、10.76～107.60 μg·ml^-1(r=0.999 8)、7.92～79.20 μg·ml^-1(r=0.999 8)范围内呈良好的线性关系,平均加样回收率分别为99.19%(RSD=0.9%)、98.44%(RSD=1.1%)、99.12%(RSD=1.0%)、99.18%(RSD=1.1%)(n=9)。结论:该方法简便、准确、重复性好,可用于黄连上清片的质量控制。     

HPLC波长切换法考察60Co辐照对地榆槐角丸中5种有效成分的影响

摘 要 目的：考察60Co辐照灭菌对地榆槐角丸中5种有效成分含量的影响。 方法: 采用HPLC法,色谱柱为Waters Sunfire ODS C18柱（250 mm×4.6 mm,5 μm）,流动相为甲醇 0.1%磷酸溶液,梯度洗脱;流速：1.0 ml·min-1;波长：210 nm、278 nm、230 nm、403 nm;柱温：30℃,进样量：10 μl,比较有效成分槐角苷、黄芩苷、梓醇、芍药苷、羟基红花黄色素A辐照前后含量的变化,并将所得数据用SPSS 22.0软件分析。 结果: 地榆槐角丸中的梓醇、芍药苷、羟基红花黄色素A、槐角苷、黄芩苷分别在0.02～0.37 μg、0.04～0.59 μg、0.11～1.68 μg、0.21～3.29 μg、0.61～9.74 μg范围内线性良好,平均加样回收率分别为101.28%,102.34%,98.42%,99.91%,100.47%,RSD分别为1.15%,1.37%,1.08%,1.63%,1.71%(n=9)。辐照剂量不超过6 kGy时,各组分含量变化无统计学意义（P＞0.05）,辐照剂量为8 kGy时,芍药苷和羟基红花黄色素A含量在辐照前后变化显著（P＜0.05）。 结论: 所建立的地榆槐角丸活性成分测定方法可作为质控方法。在60Co辐照剂量不超过6 kGy时,5种有效成分含量变化不显著,可为地榆槐角丸辐照灭菌手段提供参考。     

HPLC法测定抗601合剂中黄芩苷的含量

摘 要 目的： 建立抗601合剂中黄芩苷的含量测定方法。方法: 采用高效液相色谱法。色谱柱为Agilent Eclipse Plus C₁₈（250 mm×4.6 mm, 5 μm）,流动相为甲醇：0.1%磷酸溶液(48∶52),检测波长为280 nm,柱温为室温(25 ℃),流速为0.8 ml·min^-1,进样体积为20 μl。结果: 黄芩苷测定质量浓度在18.897～188.975 μg·mL^-1范围内与其相应峰面积积分值呈良好线性关系(r=0.999 9);平均加样回收率为99.86%,RSD为0.32% (n=9)。结论:该方法专属性、重复性、准确性好,可用于抗601合剂中黄芩苷的含量测定。     

Analgesia induced by brief footshock is inhibited by 5-hydroxytryptamine but unaffected by antagonists of 5-hydroxytryptamine or by naloxone

Exposure to footshock (1 mA) for 30 sec induced a marked analgesia that was enhanced by pretreatment with the 5HT synthesis inhibitor, p-chlorophenylalanine, and attenuated by the 5HT releasing drugs p-chloroamphetamine and fenfluramine, by the 5HT re-uptake inhibitor, fluoxetine and by the 5HT agonists, 5-methoxy-N,N-dimethyltryptamine and MK212. However, agonists, quipazine and trifluoromethylphenylpiperazine, with greated reported affinities for 5HT binding sites on rat brain membranes than MK212 were without effect as were the antagonists metergoline, methysergide, cyproheptadine, mianserine and methiothepin. The specific opioid antagonist naloxone was also without effect. The results in general indicate that analgesia induced by brief footshock (1 mA, 30 sec) is inversely related to 5HT availability but thereis little evidence of involvement of known 5HT receptors.     

Synergism by caffeine and by cocaine of the motor control deficit produced by midazolam

To evaluate the effects of caffeine and cocaine on the impairment of discriminative motor control produced by midazolam, rats were trained to hold a force transducer operated with a paw so that it remained between upper and lower limits of a force band for a continuous 1.5-s period to deliver each food pellet. Acute doses of 3 mg/kg midazolam SC impaired motor performance. Except for one animal, caffeine (10-40 mg/kg IP) had little or no effect on performance, while cocaine (3.75-22.5 mg/kg IP) produced dose-related impairment. When each dose of caffeine was combined with 3 mg/kg midazolam, a marked synergism in motor performance impairment occurred. Cocaine plus midazolam produced mainly an additive synergism. The conspicuous synergistic action of caffeine on the motor control deficit produced by midazolam contrasts with the typical antagonism found between the benzodiazepines and methylxanthines when performance is evaluated by psychomotor tests not requiring fine motor control.     

Deamination of beta-phenylethylamine by monoamine oxidase--inhibition by imipramine

The oxidative deamination of tyramine (Tyr), 5-hydroxytryptamine (5-HT), and β-phenylethylamine (PEA) by mitochondrial preparations of rabbit lung and brain was inhibited by imipramine. This tricyclic iminodibenzyl antidepressant drug was most effective in decreasing the deamination of PEA: at 1 × 10^?4M imipramine, deamination of PEA, Tyr and 5-HT was inhibited by approximately 70, 45 and 45 per cent, respectively, when either lung or brain mitochondrial monoamine oxidase (MAO) preparations were used. Imipramine-induced inhibition of MAO was shown to be of a mixed type based on Lineweaver-Burk plots, but was found to be completely reversible. The desmcthyl and didesmethyl derivatives of imipramine were equally as effective as the parent drug in inhibiting the deamination of PEA, whereas the N-oxide analog of imipramine was less effective as an inhibitor of this reaction. These results support the premise that the action of imipramine as a clinically effective antidepressive agent may be related to its inhibitory effect on the specific form of MAO which deaminates PEA.     

Augmentation by serrapeptase of tissue permeation by cefotiam

Cefotiam (CTM) is a new cephalosporin with a broad spectrum of activity against both Gram-positive and Gram-negative microorganisms. Cephalosporins are widely used for prophylaxis of infections in patients undergoing thoracotomy. Augmentation by serrapeptase on tissue permeation of CTM was examined in 35 thoracotomy patients with lung cancer. The subjects were divided into two groups according to the method of the administration of CTM. Group I consisted of 17 subjects, each of whom received a single dose of 2 g of CTM alone by an instillation for 30 minutes. Group II consisted of 18 subjects, each of whom received a combination of CTM and serrapeptase; serrapeptase was given 2 tablets (10 mg) each time for three times/day until the day before surgery, and then CTM was administered by the same procedure. The following results were obtained: Individual difference was observed for the permeation of CTM into tissues. Pathologic differences also affected the permeation. Nevertheless, the CTM levels in pulmonary tissues reached about a half of those in the blood in both the single dose group and the combination group, hence sufficient concentrations exceeding MIC80 for main microorganisms that caused infections in the lung were obtained. The concentrations of CTM in inflammatory tissues have showed lower levels than those of normal tissues in both CTM single dose and the combination groups. Decrease of blood flow volume may have contributed to the reduction in levels of CTM in the inflammatory tissues. The ratio of the concentration of the drug in pulmonary tissues to that in the blood was 29.1 +/- 2.5% in the single dose group, and 44.2 +/- 6.0% in the combination group, the latter showing quite a significant increase (P less than 0.05). Combined administrations of CTM and serrapeptase deserves more trials in the case when surgical treatments of the lung are performed. An antiinflammatory effect of serrapeptase in the respiratory system is expected, and in addition, the combined use of CTM and serrapeptase should stimulate permeation of the antibiotic into tissues.     

Interference by cephalosporins with creatinine measurement by desk-top analyzers

Summary We have carried out a study to evaluate the interference by cephalosporins with the measurement of creatinine by desk-top analyzers. The cephalosporins evaluated at concentrations of 0–250 mg/l were cefazolin sodium, cefoxitin sodium, cefotaxime sodium, and ceftazidime pentahydrate. The instruments evaluated were DT60 (Kodak, Rochester, USA), Seralyzer (Ames Division, Miles Laboratories, IN, USA), and Vision (Abbott Labs, Chicago, USA). All studies were done in plasma.None of the cephalosporins showed any interference with the DT60 analyzer. With the Vision and Seralyzer no interference was seen with cefotaxime or cefazolin. With cefazolin an increase of 10–20 µmol/l creatinine was seen for every 20 mg/l of drug; with cefoxitin there was an increase of 50–80 µmol/l of creatinine for every 100 mg/l of drug.Erroneous creatinine values may be found in patients taking cefazolin and cefoxitin and may lead to inappropriate clinical management.     

Antagonism of morphine by beta-melanocyte-stimulating hormone and by tetracosactin

Using the decerebrate—spinal Lloyd preparation morphine depressed evoked mono- and polysynaptic reflex activity, β-melanocyte-stimulating hormone enhanced monosynaptic reflex activity, and tetracosactin had no effect. When morphine injection was preceded either by β-melanocyte-stimulating hormone or by tetracosactin a statistically significant depression was not observed. The stimulant actions of β-melanocyte-stimulating hormone did not appear to account for its capacity to antagonize morphine. The fall of blood pressure which follows the administration of morphine in this preparation was not antagonized by the prior administration of either polypeptide.     

Immunomodulation by non-absorbable antibiotics given by the intragastric route

To test the role of bacterial fractions released from intestinal flora during immunomodulation by antimicrobial agents, BALB/c mice were treated with the non-absorbable antibiotics polymyxin B or teicoplanin by the intragastric route. The composition of faecal microbiota and the capacity of spleen cells to proliferate in response to B-cell and T-cell mitogens were assessed at several times during the treatment. Both antibiotics lowered the count of some bacteria of the intestinal flora and induced significant modifications in spleen cell ability to proliferate in response to mitogens. Thus, the active fractions released from intestinal bacteria during antibiotic treatments may be able to induce immunomodulating effects.