To analyze the structure of the maximum impurity in halometasone/triclosan cream and discuss the rationality of the current registered standard for imported drugs.

The related substances in halometasone/triclosan were detected according to JX20080304, and dioxins were determined according to USP. Finally, the possible structures of the maximum impurity were characterized by LC-Q TOF/MS.

The results showed that the maximum unknown impurity(RRT 0.67), calculated according to halometasone was OOS(1.0%) at 2.5%. The peak was related to triclosan through comparing with the chromatography behavior of triclosan in reference substance solution. MS information indicted the process impurities of triclosan.

For compound preparations, to ensure the stability and safety of the product, the impurities relevant to different components should be controlled separately at rational limit based on safety data.

To establish the UPLC-MS/MS method for simultaneous determination of 9 components (nicotinic acid, kaempferol, swertisin, quercetin, luteolin, rutin, vitexin, spinosin, salicylic acid) in Desmodium caudatum (Thunb.) DC. and construct a back propagation(BP) neural network model to predict the origin of Desmodium caudatum (Thunb.) DC. from different habitats.

The chromatographic separation was achieved on an Agilent Zorbax SB C₁₈ column (50 mm×3.0 mm，1.8 μm). The mobile phase consisted of methanol -0.1% acctic acid (containing 0.02 mol·L^-1 ammonium acetate) at a flow rate of 0.3 mL·min^-1 with gradient elution, the MS analysis were performed by multiple reaction monitoring (MRM) under ESI⁺ and ESI. A correlation analysis was conducted on the contents of each component, and a BP neural network model was constructed to distinguish Desmodium caudatum (Thunb.) DC. from different habitats.

Under the optimized conditions, 9 components(nicotinic acid, kaempferol, swertisin, quercetin, luteolin, rutin, vitexin, spinosin, salicylic acid) showed good linear relationships in the ranges of 0.388 8-38.88 ng·mL^-1, 10.07-1 006.6 ng·mL^-1, 34.22-34 221.6 ng·mL^-1, 3.944-394.4 ng·mL^-1, 2.124-212.4 ng·mL^-1, 4.344-434.4 ng·mL^-1, 46.50-4 650.1 ng·mL^-1, 1.649-164.9 ng·mL^-1, 4.880-488.0 ng·mL^-1, respectively (r>0.995 1), whose average recoveries were 96.9%-103.9% (RSDs<1.9%). The contents of the above nine components in 40 batches of Desmodium caudatum (Thunb.) DC. were 1.657-7.407 μg·g^-1, 15.801-64.488 μg·g^-1, 1 068.348-4 270.780 μg·g^-1, 10.608-123.228 μg·g^-1, 3.897-16.802 μg·g^-1, 1.269-97.834 μg·g^-1, 405.285-1 955.796 μg·g^-1, 13.614-36.124 μg·g^-1, 4.417-87.509 μg·g^-1, respectively. According to correlation analysis, four components (swertisin, rutin, spinosin, and luteolin) in Desmodium caudatum (Thunb.) DC. showed a highly linear positive correlation, indicating that these four components had a certain synergistic effect in Desmodium caudatum (Thunb.) DC.. The BP neural network model was constructed to predict Desmodium caudatum (Thunb.) DC. from different habitats, and the accuracy of the test set reached 92.3%.

The method is simple, sensitive and efficient, and can be used for the rapid determination of the components in Desmodium caudatum (Thunb.) DC.. Using the BP neural network model to predict the habitats plays a significant role in tracing the origin of Desmodium caudatum (Thunb.) DC..

To establish a rapid molecular identification method for DNA fingerprinting-immunocolloidal gold test strips of Chinese herbal medicine human placentophagy genetic markers and to develop an integrated quality control gene detection kit.

Self-developed method and reagents could be for template DNA extraction from human placentophagy. Species-specific primers were designed according to the human mtDNA cytb gene, and the 5’ ends of the primers were labeled with FAM and Biotin, respectively. The optimal annealing temperature and cycle number of PCR were screened to establish a DNA fingerprinting molecular identification method. To develop PCR gene detection reagent premixes, to prepare DNA clones of control herbs using molecular cloning and gene sequencing techniques and to utilize immunocolloidal gold test strips for result detection. Finally, a rapid gene detection kit integrating DNA extraction reagent, PCR gene detection reagent premixes, control herb DNA clone solution, blank control solution and test strips was developed, and evaluated for specificity, reproducibility, sensitivity and stability.

The template DNA extracted by self-developed DNA extraction reagents were all in the concentration of 150-280 ng·μL^-1, the purities were all in the range of 1.8-1.9, and there were no trail in the agarose gel electrophoresis. And the immunocolloidal gold test strips showed two red bands for human placentophagy control herb and authentic product, and one red band for easy-mix product and blank control at annealing temperature of 59 ℃ and 20 cycles for human placentophagy specific primers. The agarose gel electrophoresis was verified to be correct. The DNA sequencing results of the control herbs were 100% homologous with human mtDNA cytb gene. The self-developed integrated rapid gene detection kit was specific, reproducible, stable and sensitive at 0.1 ng·μL^-1.

The DNA fingerprinting-immunocolloidal gold test strip molecular identification method can specifically, accurately, rapidly and visually identify the authenticity of human placentophagy, and the integrated rapid gene detection kit provides a regulated and standardized testing method for quality control of human placentophagy. Therefore, it is more suitable for on-site field testing and universal promotion.

To analyze and optimize stir-baked with vinegar technology of Genkwa Flos decoction pieces by multi-index weighted scoring method based on orthogonal experiment, and to provide technical index on standardization of stir-baked with vinegar technology of Genkwa Flos decoction pieces.

The orthogonal experiment was employed to analyze and evaluate the four key factors related to stir-baked with vinegar technology including the amount of vinegar, dampening time, temperature and stir-baked time by the six main indicators including the total contents of chlorogenic acid, tiliroside, luteolin, apigenin, hydroxygenkwanin and genkwanin, the content of alcohol extractive and appearance characters.

The amount of vinegar and stir-baked temperature had notable effects, while the dampening time and stir-baked time had no notable effects on the test results. Considering comprehensively the effects of four key factors, the optimized stir-baked with vinegar technology was as follows: add 0.3 kg of vinegar to 1 kg of Genkwa Flos, and fry at 160 ℃ for 10 min after dampening for 15 min.

This study offers guidance and reference for standardizing the stir-baked with vinegar technology of Genkwa Flos decoction pieces.

To establish an HPLC-MS/MS method for the simultaneous determination of six characteristic components of Scutellariae Radix including baicalein, baicalin, wogonin, wogonoside, chrysin and oroxylin A in rat plasma, and to compare their pharmacokinetic profiles after oral administration of Scutellariae Radix and Niuhuang Jiedu tablets (NHJDT) to rats.

Rats were given 250 mg·kg^-1 of NHJDT suspension or the prescribed equivalent amount of Scutellariae Radix aqueous extract, and plasma samples were collected at different time intervals. Naringenin was used as internal standard. After precipitated with methanol, the plasma samples were separated on an Inertsil C₈-3 (150 mm×4.6 mm, 5 μm) column by linear gradient elution with 0.1% formic acid solution(A)-0.1% formic acid-methanol(B) as mobile phase. The flow rate was 1.0 mL·min^-1, and the column temperature was 35 ℃. The analytes were detected by tandem mass spectrometry with the electrospray ionization (ESI) source combined with multiple reaction monitoring(MRM) mode in positive ion mode. The pharmacokinetic parameters were calculated and statistically analyzed.

The six characteristic components of Scutellariae Radix were all in good linear relationships in the range of 5-500 ng·mL^-1. The RSDs for accuracy test were in the range of 88.43%-108.6%, and the RSDs for inter-batch and intra-batch precision tests were all below 15%. The matrix effect and plasma stability met the requirements of methodology validation in biological sample analysis. Baicalin and wogonoside were the major components detected in rat plasma after oral gavage of Scutellariae Radix aqueous extract and NHJDT suspension. The AUC_0-t of wogonoside was significantly increased in NHJDT group compared with Scutellariae Radix group. Furthermore, the C_max of wogonoside and baicalin were significantly increased while the T_max was decreased after NHJDT suspension administration.

This method is specific and sensitive for the determination of six characteristic components of Scutellariae Radix, and suitable for pharmacokinetic study of rat plasma. NHJDT with co-existing components enhances the absorption and influences the pharmacokinetic behaviors of active ingredients of Scutellariae Radix.

To explore the method of pharmacognosic identification of four medicinal seeds, such as Plantaginis Semen from two kinds of original plant，Allii Fistulosi Semen, Allii Tuberosi Semen, and to digitize the identification characteristics.

The seeds of the four medicinal plants were studied by means of type microscope and light microscope, including the appearance(positive view, bottom view, hilum view and surface feature), internal morphology(cross profile and longitudinal profile) and the characters of micromorphology(transverse section, powder). The characteristics of the four medicinal seeds were summarized, and the identification points were characterized by digital method.

The seeds of the four medicinal plants could be identified according to the appearance, internal morphology and the characters of micromorphology.

This study lays a foundation for the variety identification and provides reference for the standard formulation and quality control of the four medicinal seeds. It also provides ideas for digital characterization of seed medicinal materials.

To establish high-performance liquid chromatography method using cyclodextrin as a mobile phase additive for the determination of ursolic acid and oleanolic acid in Corni Fructus, providing a basis for quality control of Corni Fructus.

Molecular design and response surface method were used to optimize the determination method of ursolic acid and oleanolic acid in Corni Fructus. Agilent Eclipse XDB C₁₈ column (150 mm×4.6 mm, 5 μm) was adopted as the stationary phase, the mobile phase was 3 mmol·L^-1 γ-cyclodextrin solution (contained 0.05% phosphoric acid)-acetonitrile (60∶40), the flow rate was 1.0 mL·min^-1, the column temperature was 25 ℃ and the detecting wavelength was 210 nm.

The resolution of chromatographic peaks of ursolic acid and oleanolic acid was 3.81. Linearities were good in the range of 400-4 000 ng for ursolic acid and in the range of 200-2 000 ng for oleanolic acid. The RSDs for precision, reproducibility, and stability were less than 1.4%, 1.8%, and 1.7%, respectively. The recovery rates were 98.5% (RSD=1.7%) and 99.1% (RSD=2.0%). The contents of ursolic acid in three batches of Corni Fructus were 2.66 mg·g^-1, 2.35 mg·g^-1 and 2.91 mg·g^-1, and those of oleanolic acid were 0.83 mg·g^-1, 0.78 mg·g^-1and 1.12 mg·g^-1, respectively.

This method is simple, accurate, reliable, and environmental friendly, and can be used as a quality control for Corni Fructus.

To establish a quantitative analysis of multi-components by single marker (QAMS) method for the simultaneous determination of nine effective components including phenolic acids and flavonoids (neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, rutoside, isoquercitrin, kaemperol-3-O-rutinoside, 3，4-O-dicaffeoylquinic acid, 3，5-O-dicaffeoylquinic acid, 4，5-O-dicaffeoylquinic acid), in Solidaginis Herba.

Ultra-high performance liquid chromatography was developed on an ACQUITY UPLC^® HSS T3 (100 mm×2.1 mm, 1.8 μm) column with acetonitrile (A)-0.1% phosphoric acid solution (B) as mobile phase in gradient elution. The flow rate was 0.3 mL·min^-1, the detection wavelength was 327 nm, the column temperature was 30 ℃, and the injection volume was 1 μL. Chlorogenic acid and rutoside were chosen as the internal standards for phenolic acids and flavonoids respectively to establish the determine correction factors of neochlorogenic acid, cryptochlorogenic acid，3，4-O-dicaffeoylquinic acid, 3，5-O-dicaffeoylquinic acid, 4，5-O-dicaffeoylquinic acid isoquercitrin and kaemperol-3-O-rutinoside, respectively, by multi-point correction method and their contents were calculated. The results were compared with the results of external standard method to verify their accuracy.

Nine components showed good linear relationships within their own ranges(r≥0.999 5), whose average recoveries were 98.2%-101.7% with the RSDs of 1.0%-1.7%. The contents of neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, rutoside, isoquercitrin, kaemperol-3-O-rutinoside, 3，4-O-dicaffeoylquinic acid, 3，5-O-dicaffeoylquinic acid and 4，5-O-dicaffeoylquinic acid, in nine batches of samples were 0.008%-0.014%, 0.055%-0.097%, 0.010%-0.019%, 0.191%-0.412%, 0.018%-0.035%, 0.116%-0.50%, 0.028%-0.048%, 0.111%-0.235% and 0.113%-0.182%. The results obtained by QAMS were consistent with those of external standard method(relative average deviations less than 2.8%).

The simple, accurate and reproducible method can be used for the quality control of Solidaginis Herba.

To establish a solid-phase extraction-high performance liquid chromatography(SPE-HPLC) method for the rapid detection of related substances of vitamin D₃, trans vitamin D₃ (impurity A), 7-dehydrocholesterol (impurity B), lumisterol 3 (impurity C), and isotachysterol 3 (impurity D), in vitamin D drops (soft capsules).

The content, which was approximately equivalent to vitamin D₃ 1 548 IU, was taken in about 1.2 g, weighed accurately, put into a test tube, 4 mL of isooctane was added to it, and it was swirled and mixed well. Purification was performed using solid phase extraction columns, with n-hexane-ethyl acetate(85∶15) as the elution agent and anhydrous ethanol as the desorption agent. A Luna Silica(2) 100 Å silica gel column(150 mm×4.6 mm, 3 μm) was used, with n-hexane-n-pentanol (996.5∶3.5) as the mobile phase. The content of vitamin D₃ impurities was calculated using the adding standard calibration factors principal component self-control method.

The separation degree between pre-vitamin D₃ and vegetable oil was greater than 1.5. The linear range of vitamin D₃ was 0.02-0.80 μg·mL^-1, with r=0.999 5. The linear range of impurity A was 0.02 -0.80 μg·mL^-1, with r=0.999 9. The linear range of impurity B was 0.02-0.80 μg·mL^-1, with r=0.999 9. The linear range of impurity C was 0.02-0.80 μg·mL^-1, with r=0.999 9. The linear range of impurity D was 0.02-0.80 μg·mL^-1, with r=0.999 9. The average recovery rate of impurities A-D (n=9) was 93.2%-102.9%. The detection results of 3 batches of vitamin D drops (soft capsules) showed that the content of known impurities and other maximum single impurities were less than 0.5%, and the total content of impurities was less than 1.0%.

The results indicate that the established method is suitable for the detection of vitamin D₃ related substances in vitamin D drops (soft capsules). It has the advantages of being easy to operate, providing rapid and accurate results, and providing technical assurance for the quality control of fat-soluble vitamin D₃ preparations.