Contribution of momilactones A and B to diabetes inhibitory potential of rice bran: Evidence from in vitro assays

This study was the first to detect the presence of the two compounds momilactone A (MA) and momilactone B (MB) in rice bran using liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS). By in vitro assays, both MA and MB exhibited potent inhibitory activities on pancreatic α-amylase and α-glucosidase which were significantly higher than γ-oryzanol, a well-known diabetes inhibitor. Remarkably, MA and MB indicated an effective inhibition on trypsin with the IC₅₀ values of 921.55 and 884.03 µg/mL, respectively. By high-performance liquid chromatography (HPLC), quantities of MA (6.65 µg/g dry weight) and MB (6.24 µg/g dry weight) in rice bran were determined. Findings of this study revealed the α-amylase, α-glucosidase and trypsin inhibitors MA and MB contributed an active role to the diabetes inhibitory potential of rice bran.     

液质联用技术鉴定清血八味片化学成分研究

目的:采用高效液相色谱-三重四级杆质谱(HPLC-MS/MS)测定清血八味片中的化学成分。方法:在负离子条件下采用Halo C_(18)色谱柱(2.1 mm×100 mm,2.7μm),以0.1%甲酸-10 mmol/L甲酸铵水和乙腈为流动相进行梯度洗脱,质谱采用Scan模式和MRM模式,检测清血八味片中的化学成分。结果:共鉴定出紫草中成分7种、土木香中成分3种、人工牛黄中成分4种、栀子中成分7种、瞿麦中成分7种、甘草中成分12种。结论:该方法快速可靠,操作简便,可用于清血八味片的质量控制研究,为临床药物使用提供一定的依据。     

三七HPLC指纹图谱及5种成分测定

目的 建立三七HPLC指纹图谱,并测定5种成分的含有量.方法 三七70%甲醇提取物的分析采用Waters XBridge C18色谱柱(4.6 mm×250 mm,5μm);流动相乙腈-水,梯度洗脱;体积流量1.5 mL/min;柱温25℃;检测波长203 nm.结果 15批样品指纹图谱中有5个共有峰,相似度均大于0.99.三七皂苷R1、人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1和人参皂苷Rd分别在0.000 76~0.567 64(r=0.9999)、0.002 69~2.017 43 (r=0.9998)、0.000 38~0.283 82 (r=1.000 0)、0.002 83~2.12483 (r=0.999 8)、0.000 78~0.582 98 mg/mL (r=0.999 8)范围内线性关系良好,平均加样回收率分别为101.78%、97.22%、102.14%、98.96%、101.73%,RSD分别为1.58%、1.31%、2.17%、1.55%、1.80%.结论 该方法简便、快速、准确,可用于三七的质量控制.     

四种大宗常用中药饮片中黄曲霉毒素污染状况分布比较研究

目的 测定不同来源的4种大宗常用中药饮片中黄曲霉毒素（AFB₁、AFB₂、AFG₁和AFG₂）的含量，比较不同基质中药饮片中黄曲霉毒素的分布状况。方法 基于免疫亲和柱净化-高效液相色谱分离-荧光检测器（IAC-HPLC-FLD）方法，分析不同产地共75批中药样品。结果 柏子仁、薏苡仁、决明子及党参共计75批中药饮片中，阳性检出：26批柏子仁（AFs 1.22-46.67 μg·kg^-1，AFB₁ 1.22-31.40 μg·kg^-1）、4批薏苡仁（AFs 1.97-41.13 μg·kg^-1，AFB₁ 1.97-36.40 μg·kg^-1）、1批决明子（AFs 13.65 μg·kg^-1，AFB₁ 12.60 μg·kg^-1），阳性率41%，超标率15%。阳性样品经 LC-MS/MS确证，排除假阳性。4种大宗常用中药饮片柏子仁、薏苡仁、决明子、党参中黄曲霉毒素的污染水平依次降低，阳性检出率分别为77%、29%、7%、0%，表明中药材中黄曲霉毒素的污染状况与药材基质密切相关。结论 针对易污染AFs的中药品种，需进一步加强其污染状况的全面检测分析，为黄曲霉毒素的有效防控以及完善中药的质量标准提供科学依据，从而保障中药用药安全。     

HPLC法同时测定外感风寒颗粒中10种成分

目的建立HPLC法同时测定外感风寒颗粒(桂枝、防风、葛根等)中苦杏仁苷、3’-羟基葛根素、葛根素、3’-甲氧基葛根素、升麻素苷、升麻素、5-O-甲基维斯阿米醇苷、亥茅酚苷、肉桂酸、桂皮醛的含有量。方法该药物甲醇提取液的分析采用Agilent ZORBAX Eclipse XDB-C18色谱柱(4.6 mm×250 mm,5μm);流动相乙腈-0.1%磷酸,梯度洗脱;体积流量1.0 m L/min;柱温25℃;检测波长207、254、280 nm。结果 10种成分在各自范围内线性关系良好(r≥0.999 1),平均加样回收率为96.97%~100.08%,RSD为0.80%~1.45%。结论该方法简便、重复性好,可用于外感风寒颗粒的质量控制。     

车前子酒炙工艺优选及其不同炮制品对比研究

[目的] 优选酒炙车前子的最佳炮制工艺，并对车前子生品、酒炙品、盐炙品进行对比研究。[方法] 以车前子中京尼平苷酸和毛蕊花糖苷的含量为考察指标，选择加酒量、闷润时间、炒制温度、炒制时间为考察因素，通过单因素实验优选车前子的最佳酒炙工艺。采用高效液相色谱-二极管阵列检测器（HPLC-DAD）建立车前子水提液指纹图谱测定方法，通过指标成分含量、不同炮制品水提液的出膏率及指纹图谱相似度分析不同炮制品间的差异。[结果] 酒炙车前子的最佳炮制工艺为每100 g车前子加黄酒10 g，闷润60 min，150℃下炒制9 min。经盐炙和酒炙后，车前子中的京尼平苷酸和毛蕊花糖苷的含量均较生品显著增加，而两种炮制品并无统计学差异；在出膏率方面，盐炙和酒炙车前子的出膏率无明显差异，但均高于生车前子。高效液相色谱（HPLC）指纹图谱显示车前子生品、盐炙品和酒炙品具有很好的相似度。[结论] 优选出的车前子酒炙工艺稳定可行，并与盐车前子在成分上具有一致性，鉴于酒车前子已不再流通，在经典名方的开发研究中，可考虑用现行通用的盐车前子取代。     

Development and validation of ultra-performance liquid chromatography method for the determination of meloxicam and its impurities in active pharmaceutical ingredients

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The Selection of a Pharmaceutical Salt—The Effect of the Acidity of the Counterion on Its Solubility and Potential Biopharmaceutical Performance

A roadmap for the selection of a pharmaceutical salt form for a development candidate is presented. The free base of the candidate did not have sufficient chemical stability for development. The initially selected salt form turned out to be undevelopable because it was unstable during scale-up synthesis and storage. The rationale for the new solid form screening and the criteria for selection are discussed. Before the final selection, the pH solubility profiles of the 2 new salts, a benzoate and a besylate, were compared. Atypical solubility behavior was observed for the benzoate salt in hydrochloric acid with and without normal saline. A scheme is proposed illustrating how the pKas of the counterion and active pharmaceutical ingredient, the medium composition, and final pH affect the solubility and solution equilibria of the 2 selected salt forms. This scheme also includes the equilibria between solution and solid phases in different pH ranges. The pharmaceutical importance of this research is that it sheds light on how the acidity of the counterion can affect the solubility of the selected salt form in the gastric environment. With a well-designed formulation strategy, this property potentially can be translated to optimal biopharmaceutical performance of the drug product.     

Preparation and Quality Evaluation of Salvianolic Acids and Tanshinones Dry Powder Inhalation

Salvianolic acids and tanshinones both exhibit efficacy in treating idiopathic pulmonary fibrosis (IPF), but their formulation limits their clinical use. This study aimed to prepare the salvianolic acids and tanshinones dry powder for inhalation (SPI) to achieve pulmonary delivery for the treatment of IPF. The variable quantities of salvianolic acids and tanshinones composite powder were optimized using the central composite design-response surface method. Different carriers with various drug-carrier ratios were optimized to prepare SPI. The final optimized formulation of SPI was as follows: InhaLac 230^® was selected as the carrier with drug:carrier = 1:6, and the milled lactose InhaLac 400^® was added at 5%. The developed SPI characterized with an angle of repose 52.46 ± 1.04°, Carr's index of 34.00 ± 0.50% and showed high lung deposition in vitro, indicating the potential of pulmonary delivery for the treatment of IPF.     

Bottom-Up and Top-Down Approaches to Explore Sodium Dodecyl Sulfate and Soluplus on the Crystallization Inhibition and Dissolution of Felodipine Extrudates

The objectives of this study were to explore sodium dodecyl sulfate (SDS) and Soluplus on the crystallization inhibition and dissolution of felodipine (FLDP) extrudates by bottom-up and top-down approaches. FLDP extrudates with Soluplus and SDS were prepared by hot melt extrusion, and characterized by polarized light microscopy, differential scanning calorimetry, and fourier transform infrared spectroscopy. Results indicated that Soluplus inhibited FLDP crystallization, and the whole amorphous solid dispersions (ASDs) were binary FLDP-Soluplus (1:3) and ternary FLDP-Soluplus-SDS (1:2:0.15～0.3 and 1:3:0.2～0.4) extrudates. Internal SDS (5%-10%) decreased glass transition temperatures of FLDP-Soluplus-SDS ternary ASDs without presenting molecular interactions with FLDP or Soluplus. The enhanced dissolution rate of binary or ternary Soluplus-rich ASDs in the nonsink condition of 0.05% SDS was achieved. Bottom-up approach indicated that Soluplus was a much stronger crystal inhibitor to the supersaturated FLDP in solutions than SDS. Top-down approach demonstrated that SDS enhanced the dissolution of Soluplus-rich ASDs via wettability and complexation with Soluplus to accelerate the medium uptake and erosion kinetics of extrudates, but induced FLDP recrystallization and resulted in incomplete dissolution of FLDP-rich extrudates. In conclusion, top-down approach is a promising strategy to explore the mechanisms of ASDs' dissolution, and small amount of SDS enhances the dissolution rate of polymer-rich ASDs in the nonsink condition.