双波长HPLC法测定止痒地霜中地塞米松和羟苯乙酯的含量

目的 建立双波长HPLC法同时测定止痒地霜中地塞米松磷酸钠和羟苯乙酯的含量。方法 采用RP-HPLC法,以Wondasil C₁₈（4.6 mm×250 mm,5 μm）为色谱柱,以三乙胺溶液-甲醇-乙腈（52：43：5）为流动相;检测波长为242 nm,流速为1.0 ml/min。结果 羟苯乙酯和地塞米松磷酸酯分别在21.42～64.26 μg/ml （r=1.0000）和20.84～62.53 μg/ml （r=0.9999）范围内有良好的线性关系,平均回收率分别为99.1%（RSD=0.41%）和99.0%（RSD=0.72%）。结论 该法简便、准确、重复性好,可用于止痒地霜的质量控制。     

UHPLC法同时测定铁苋菜中4种成分含量

目的 采用UHPLC法构建铁苋菜中没食子酸,原儿茶酸,没食子酸甲酯,芦丁等4种成分的含量测定方法。方法 固定相为Poroshell 120 SB-C₁₈ (3.0 mm×150 mm,2.7 μm)色谱柱;流动相为A相0.1%甲酸-水,B相0.1%甲酸-乙腈,梯度洗脱（0~3 min,5%B→10%B;3~5 min,10%B→25%B;5~10 min,25%B→30%B）柱温40 ℃,流速0.6 mL·min^-1,检测波长265 nm。结果 4种成分的线性关系良好,平均加样回收率为100.5%~100.9%,RSD 均小于3.0%;10批样品中4种成分的含量分别为0.27~0.71,0.57~1.64,2.15~4.36,0.53~1.65 mg·g^-1。结论 该方法简便高效,稳定准确,有助于铁苋菜药材的全面质量控制。     

UPLC波长切换法同时测定小陷胸汤中4种指标性成分的含量

目的 基于UPLC波长切换法构建小陷胸汤中腺苷,巴马汀,小檗碱,葫芦素B等4种指标性成分的含量测定方法。方法 固定相为Poroshell 120 EC-C₁₈ (3.0 mm×150 mm,2.7 μm)色谱柱;流动相为A相为0.1%甲酸-水,B相为0.1%甲酸-乙腈,梯度洗脱（0~6 min,B：5%→8%;6~9 min,B：8%→35%;9~12 min,B：35%→50%）,检测波长0~10 min,262 nm;10~12 min,234 nm,柱温46℃,流速0.6 mL·min^-1。结果 小陷胸汤中4个成分腺苷、巴马汀、小檗碱、葫芦素B分别在0.017～0.17,0.073～0.73,0.15～1.50 ,0.01～0.10 mg?mL^-1范围内呈良好线性关系;平均加样回收率分别为100.0%、100.6%、101.2%、99.1%,RSD均小于3.0%（n=6）;4种成分的含量分别为0.052~0.061、0.24~0.30、0.49~0.59、0.033~0.045 mg?g^-1。结论 该方法精密度高、重复性好、稳定性好、简便高效,可用于小陷胸汤的质量控制。     

环酯红霉素纳米晶的大鼠肺部喷雾给药药动学研究

目的研究环酯红霉素纳米晶肺部给药的药动学,考察其肺部给药特点。方法建立液相色谱-串联质谱（LC-MS/MS）法检测环酯红霉素血药浓度,并进行专属性、精密度、准确度和稳定性、提取回收率考察;SD大鼠随机分为3组,分别以15 mg/kg iv环酯红霉素注射液、肺部喷雾给予环酯红霉素原料药和环酯红霉素纳米混悬液,于给药后0.033、0.083、0.167、0.25、0.5、0.75、1、1.5、2、3、4、6、8 h眼眶取血,检测大鼠血浆中环酯红霉素的含量,评价纳米晶对环酯红霉素肺部给药药动学、生物利用度的影响。结果色谱柱为ACQUITY UPLC HSS T3 1.8 μm（100 mm×2.1 mm）;流动相为5 mmol/L乙酸铵溶液（0.02%甲酸）-甲醇（0.02%甲酸）（85：15）;体积流量0.3 mL/min;采用电喷雾离子源（ESI）,正离子模式多反应监测（MRM）,建立的LC-MS/MS分析方法符合方法学要求。环酯红霉素以15 mg/kg iv给药后,达峰时间为0.03 h,C_max为（2 148.22±448.5） ng/mL,AUC_0-t为（660.21±96.47） h·μg/mL。环酯红霉素原料药肺部给药后,达峰时间为0.09 h,与iv给药相当,而C_max（231.54±177.19） ng/mL和_0-t 29.37±27.08） h·μg/mL较iv组显著降低（P<0.05）,其绝对生物利用度仅为3.72%。纳米晶肺部给药后,达峰时间为0.14 h,与原料药iv给药相比显著延长（P<0.05）;纳米晶肺部给药的C_max为（1 958.34±1 209.41） ng/mL,AUC_0-t为（773.11±473.49） h·μg/mL,均与iv给药相当,而显著高于原料药肺部给药（P<0.05）;其绝对生物利用度为117.10%。结论大鼠肺部给药环酯红霉素纳米晶后可明显提高环酯红霉素的生物利用度,提示纳米晶用于肺部制剂的可行性。     

HPLC-DAD法同时测定七珍汤散（努布炖屯汤）中4个成分

目的： 建立HPLC-DAD法同时测定七珍汤散中没食子酸、6-姜辣素、异土木香内酯、土木香内酯的含量,为七珍汤散的质量控制研究、考察其处方各味藏药材的成分和质量标准的提高提供参考。方法： 采用Luna C₁₈色谱柱（4.6 mm×250 mm,5μm）,流动相乙腈-0.2%醋酸溶液,梯度洗脱（0~10min,2%→12% A;10~20 min,12%→50% A;20~30 min,50%→85% A;30~50 min,85%→2% A）,流速1.0 mL·min^-1,柱温35℃,检测波长230、280 nm。结果： 4种成分实现完全分离;没食子酸、6-姜辣素、异土木香内酯、土木香内酯的线性范围依次分别在7.42~148.4、0.92~18.4、1.83~91.25、1.71~85.30 μg（r ≥ 0.9990）;平均加样回收率依次分别为99.06%、99.27%、99.86%、99.36%,RSD依次分别为1.33%、0.67%、0.35%、0.18%。结论： 该方法对4个成分同时测定,简便准确,重复性好,灵敏度高,阴性试验无干扰,可用于七珍汤散的质量控制。     

HPLC法测定黄连上清片中连翘酯苷A的含量

目的 采用高效液相色谱法测定黄连上清片中连翘酯苷A的含量。方法 色谱柱：VP-ODSC₁₈色谱柱（4.6 mm×250 mm,5 μm）,流动相：乙腈-0.4%冰醋酸溶液（15:85）,流速1.0 mL·min^-1,检测波长330 nm。结果 连翘酯苷A在10.24 ~81.92 µg·mL^-1范围内与峰面积线性关系良好(r=0.999 8),精密度试验RSD为0.85%,重复性试验RSD为1.14%,平均回收率为97.91%,RSD为1.55%(n=6)。结论 该方法操作简单,精密度良好,结果准确可靠,适用于黄连上清片中连翘酯苷A的含量测定。     

应用高效液相色谱法测定中药奇蒿中异泽兰黄素和奇蒿黄酮的含量

目的 采用高效液相色谱(HPLC)法测定中药奇蒿中异泽兰黄素和奇蒿黄酮的含量。方法 奇蒿药材以10倍体积甲醇超声60 min提取。色谱分离采用资生堂MG-C₁₈色谱柱(3.0 mm×100 mm,3μm),流动相为乙腈-0.1%甲酸(40:60,V/V),等度洗脱,流速0.5 ml/min,检测波长350 nm,柱温25℃,进样量5μl。结果 异泽兰黄素和奇蒿黄酮在15 min内基线分离,线性良好。方法学验证表明,日内、日间精密度,重复性和稳定性的范围均符合相关标准。异泽兰黄素的低、中、高加样回收率分别为100.26%,99.58%和102.24%;奇蒿黄酮的低、中、高加样回收率分别为99.09%,101.12%和101.43%。结论 该方法快捷简单,稳定可靠,可用于对奇蒿药材进行质量控制。     

HPLC法测定积雪草配方颗粒中羟基积雪草苷和积雪草苷含量

目的 建立积雪草配方颗粒中羟基积雪草苷和积雪草苷的HPLC含量测定方法。方法 色谱柱为UltimateAQ-C₁₈ 柱（4.6 mm×250 mm,5 μm）,以乙腈（A）-2 mmol/Lβ-环糊精溶液为流动相进行梯度洗脱（0~30 min： 21% A→23% A;30~60 min：23% A→25% A）,流速1.0 ml/min,柱温30 ℃,检测波长205 nm。结果 羟基积雪草苷和积雪草苷分别在0.187 7~3.754 μg和0.184 3~3.686 μg范围内与峰面积呈良好的线性关系（r>0.999 5）。经专属性、重复性、精密度、加样回收率、稳定性实验,结果均符合《中华人民共和国药典（2015年版）》方法验证的要求。结论 该含量测定方法适用于积雪草配方颗粒中羟基积雪草苷和积雪草苷的含量检测。     

HPLC法测定皮肤病血毒片中7种成分的含量

目的 建立同时测定皮肤病血毒片中7种成分含量的HPLC方法。方法 采用Kromasil C₁₈ 柱（250 mm×4.6 mm,5 μm）;流动相：乙腈-0.5%磷酸水溶液,梯度洗脱法;流速：0.8 ml/min;PDA检测器,检测波长：245、325、403 nm。结果 皮肤病血毒片中绿原酸、羟基红花色素A、芍药苷、连翘酯苷A、阿魏酸、小檗碱和甘草酸分别在10.00~200.00,4.00~80.00,20.00~400.00,4.00~80.00,3.00~60.00,10.00~200.00和10.00~200.00 μg/ml范围内呈良好的线性关系;各成分平均回收率均在95%~105%之间,RSD<2%。10批制剂中绿原酸、羟基红花色素A、芍药苷、连翘酯苷A、阿魏酸、小檗碱和甘草酸的平均含量（mg/片）与RSD（%）分别为0.299 5,2.25;0.700 0,1.33;0.429 2,1.21;0.039 1,2.34;0.014 8,2.23;0.209 0,2.06和0.272 7,2.68。结论 该方法准确可靠、简便快速,适用于皮肤病血毒片的质量控制。     

HILIC-ELSD法测定岩藻聚糖硫酸酯中岩藻糖

目的 建立一种简便、高效、准确的测定岩藻聚糖硫酸酯中岩藻糖的方法。方法 采用超声处理(300 W 100%,20 ℃,20 min);三氟乙酸(4 mol/mL)水解(110 ℃、2 h);亲水作用色谱-蒸发光检测(HILIC-ELSD)法检测,Waters XBridge^TM Amide(150 mm×4.6 mm,3.5 μm)色谱柱,流动相为乙腈-水-氨水(90:10:0.2),体积流量1 mL/min,柱温60 ℃。结果 岩藻糖的线性范围为0.100 4~1.004 mg/mL(r=0.999 4),平均加样回收率95.22%(n=6,RSD=1.16%)。结论 该方法简便、快速、准确,为岩藻聚糖硫酸酯的定量分析和质量评价研究提供了依据。     

Percutaneous penetration of octyl salicylate from representative sunscreen formulations through human skin in vitro

The human skin penetration of [¹⁴C]octyl salicylate from two representative sunscreen vehicles was determined in vitro. ³H-sucrose was incorporated into all formulations and provided a marker for membrane integrity. When applied as a finite dose in an oil-in-water emulsion vehicle containing 5% (w/w) octyl salicylate, the average total absorption of ¹⁴C over 48 hr was 0.65 ± 0.16% of the applied dose (representing a total amount permeated of 1.58 ± 0.36 μg/cm²). When applied as an infinite dose in the oil-in-water emulsion vehicle the average total absorption of ¹⁴C over 48 hr was 0.47 ± 0.22% of the applied dose (representing a total amount permeated of 27.54 ± 13.91 μg/cm²). When applied as a finite dose in a representative hydroalcoholic formulation containing 5% (w/w) octyl salicylate, the average total absorption of ¹⁴C over 48 hr was 0.59 ± 0.09% of the applied dose (representing a total amount permeated of 1.58 ± 0.25 μg/cm²). When applied as an infinite dose in the hydroalcoholic formulation the average total absorption of ¹⁴C over 48 hr was 0.23 ± 0.05% of the applied dose (representing a total amount permeated of 11.28 ± 2.55 μg/cm²). The penetration of [¹⁴C]salicylic acid [applied at a concentration of 2.7% (w/w), in the oil-in-water emulsion] was also determined. When applied as a finite dose the average total absorption of ¹⁴C over 48 hr was 1.14 ± 0.23% of the applied dose (representing a total amount permeated of 1.65 ± 0.39 μg/cm²). These results suggest that the in vitro human skin permeation of octyl salicylate is relatively low. The amounts of octyl salicylate and salicylic acid permeated when applied in similar vehicles were remarkably similar over 48 hr (1.58 μg/cm² and 1.65 μg/cm², respectively). This suggests the possibility that the ¹⁴C label appearing in the receptor fluid may, in both cases, represent salicylic acid. If this is the case, then it is possible that the amount of octyl salicylate permeating through the skin is much less than that suggested by the data obtained here. This supposition is, however, entirely speculative and has yet to be confirmed experimentally.     

3,4,5-三甲氧基苯甲酸-8-(二乙胺基)-辛酯对大鼠脑血流及其自动调节功能的影响

用激光多谱勒血流仪连续测量脑血流量（CBF），观察3,4,5-三甲氧基苯甲酸-8-(二乙胺基)-辛酯(TMB-8)对麻醉大鼠CBF及脑血流自动调节功能的影响. 结果表明, TMB-8 0.5, 1.0和2.0 mg·kg^-1呈剂量依赖性地增加CBF 5%, 20% 和34%. 其中仅2.0 mg·kg^-1组使平均动脉压（MABP）降低6%. 而尼莫地平(Nim)0.01 mg·kg^-1在使CBF增加21%的同时，使MABP降低了27%. 麻醉大鼠脑血流自动调节的MABP低限是5.3 kPa. 在MABP 4.0 kPa时TMB- 8 2.0 mg·kg^-1能增加脑血流自动调节能力，而Nim 0.01 mg·kg^-1则无明显作用. 提示TMB-8增加CBF和增强脑血流自动调节能力是其抗脑缺血作用的机理之一.     

Poly-epsilon-caprolactone nanocapsules containing octyl methoxycinnamate: preparation and characterization

This study investigates the different nanocapsules (NCs) made of poly-epsilon-caprolactone (PCL) containing the lipophilic sunscreen Escalol 557 [octyl methoxycinnamate (OMC)] and analyzes the influence of nanoparticle-based systems on light-induced decomposition of the sunscreen agent. The NCs were designed and prepared by the solvent displacement method. Formulation parameters, such as the nature and volume of the organic and aqueous phase and the nature and concentration of the surfactants and polymer, have relevant implications on NC elaboration. We investigated the influence of several technological (stirring speed: 300-800 rpm) and formulation factors [polymer amount, 195-244.5 mg; surfactant, Tween 85 (Polysorbate 85), Montanox 80 (Polysorbate 80), and Synperonic PE/F68 (Poloxamer 188) as stabilizing agents; and volume of the organic phase, 20-30 mL of acetone] on the particle size and the OMC loading capacity of the formulations--encapsulation efficiency and yield. The sizes of NC obtained were in the range of 309 to 1042 nm, the encapsulation efficiencies ranged from 93.82% to 99.97%, and yields of NC encapsulation ranged from 48.12% to 86.28%. Of all the preset experimental conditions, Montanox 80, 30 mL of acetone, 244.5 mg of polymer, and a stirring speed of 350 rpm have been selected as the best in this experimental design study. The experimental conditions selected to obtain OMC-loaded NC of 374 nm resulted in a high entrapment percentage (97.52%) and yield (82.95%). The PCL nanoparticles loaded with OMC were effective in reducing light-induced degradation of the sunscreen agent.     

萘普生的葡辛胺拆分工艺研究

对萘普生拆分中的成盐溶剂选择、左旋酸的消旋、葡辛胺的精制等３个关键问题进行了实验室研究，使拆分收率、产品质量显著提高，同时降低了拆分剂葡辛胺的消耗     

The pharmacologic activity of p-substituted DL-2-phenylglycine octyl esters

DL-2-phenylglycine octyl ester has antiphlogistic, analgesic and spasmolytic activities as shown in different animal models. The antiphlogistic effectiveness is changed only a little by the p-substitution at the phenyl ring, whereas the analgesic action is markedly influenced. Most of the substituted compounds are significantly more active than the unsubstituted ester. DL-2-(benzyloxyphenyl)glycine octyl ester is the most active compound, it has furthermore the highest therapeutic quotient. Using the i.p. application its efficacy exceeds that of acetylsalicylic acid, phenylbutazone and indometacin, respectively. The spasmolytic activity is differently changed by the substituents. The most active ester, DL-2-(p-methoxyphenyl)glycine octyl ester, is about two times more active than papaverine. In histamine induced spasm the effectiveness is low compared with the specific antagonist mepyramine. The results obtained show that the activities of the p-substituted DL-2-phenylglycine octyl esters are different with regard to the three investigated pharmacological properties.     

Antiviral effect of octyl gallate against DNA and RNA viruses

The effects of gallic acid (3,4,5-trihydroxybenzoic acid) and its alkyl esters on virus growth and virion infectivity were examined. All the compounds tested showed an inhibitory effect on the growth of herpes simplex virus type 1 (HSV-1) in HEp-2 or Vero cells. The antiviral activity of gallic acid alkyl esters was enhanced by increasing the number of carbon in the alkyl moieties of the compounds, reaching maximum at a carbon number of 12 (lauryl gallate), but both cytocidal activity and cytopathic effect of the compounds were also significantly increased simultaneously. Among these compounds, octyl gallate showed a marked antiviral effect with a relatively moderate cytotoxity. In addition, octyl gallate suppressed the multiplication of RNA viruses, such as vesicular stomatitis virus and poliovirus. Quantitative characterization of the HSV-1 infection in the presence of octyl gallate revealed that: (1) this reagent can directly inactivate HSV-1 (virucidal activity), (2) it suppresses both the intracellar multiplication and the release of the virus, (3) it selectively accelerates death of the virus-infected cells and (4) the addition of the reagent even at 6-h post infection completely abolishes the formation of progeny virus in the infected cells.     

Influence of encapsulation on the in vitro percutaneous absorption of octyl methoxycinnamate

The purpose of this study was to evaluate the in vitro transdermal permeation and skin accumulation of one ultraviolet (UV) absorber-octyl methoxycinnamate (OMC)-through pig skin and to determine the quantity of OMC in the skin surface and different pig skin layers (stratum corneum, viable epidermis, dermis, and receptor fluid). Four cases have been considered: the application of oil-in-water (O/W) and water-in-oil (W/O) emulsions containing the same filter free and encapsulated in nanocapsules (NC). The influence of the carrier on the percutaneous penetration was studied. Data showed that UV absorber exhibited increases in skin accumulation when is formulated in emulsions in free form. Skin accumulation of OMC-free in the emulsions was significantly (P < 0.05) greater than that of OMC-encapsulated for all formulations investigated. OMC-free skin accumulation ranged from 127.8 +/- 22.8 microg/cm(2) (O/W emulsion) to 172.1 +/- 12.9 microg/cm(2) (W/O emulsion). OMC-encapsulated skin accumulation ranged from 50.3 +/- 13.1 microg/cm(2) to 43.0 +/- 6.5 microg/cm(2) at NC-O/W and NC-W/O, respectively. No significant differences were found in the transdermal permeation of cinnamate for any of the formulations tested. The results of this study demonstrate that the inclusion of OMC-encapsulated in sunscreen formulations decreases the skin accumulation of the cinnamate since the in vitro release mechanism of OMC-nanocapsules is governed by hydrophobicity and crystallinity of the polymer and by the high lipophilicity of the drug. The crystallinity of the polymer have the ability of reflecting and scattering UV radiation on their own thus leading to photoprotection without the need for molecular sunscreens.     

Enteral absorption and biotransformation of the food additive octyl gallate in the rat

Following oral administration or ¹⁴C-labelled octyl gallate in a single dose of 15 mg/kg to female rats, only 20–30% of the radioactivity administered was detected in the tissues, while 60–80% of the dose was found in the contents of the gastro-intestinal tract up to 12 hr after administration. Isotope dilution analysis demonstrated the presence of the unchanged ester in the tissues. In the liver, the highest concentration of the ester demonstrated was 1·6 μg/g, in a rat killed 10 min after treatment. In the 24 hr following ip administration of labelled octyl gallate. about 91% of the administered radioactivity was recovered. Most of this was in the form of metabolites, only 9% being accounted for as unchanged ester.     

Evaluation of ibuprofen dimethyl aminoethanol octyl bromide and related active metabolites in biological samples

AF 150 is ibuprofen dimethyl aminoethanol octyl bromide, endowed with antibacterial and antiinflammatory activities. An indirect HPLC analytical method for AF 150 with UV detection, to be used for pharmacokinetic studies, has been validated in terms of linearity, reproducibility, specificity and sensitivity. Using this method the bioavailability of AF 150 and its active metabolite ibuprofen was investigated following parenteral administration and topical application.