To establish a hydrogen nuclear magnetic quantitative method which can rapidly determine the contents of linalool and protocatechuate in Homalomena occulta.

Using dimethyl sulfoxide-d₆（DMSO-d₆）as the test solvent and pyrazine -as the internal standard, ¹H-q NMR measurement was performed on a 400 MHz spectrometer. The quantitative resonance peaks of pyrazine, Linalool and protocatechuate were δ 8.66, δ 5.90 and δ 8.60, respectively.

The linear correlation coefficients of linalool and protocatechuate were good with r of 0.999 7 and 0.998 6, respectively. The RSDs of precision were 0.30% and 0.40%, and the recoveries were 98.8%-100.7%（RSD=3.7%） and 99.4%-100.6%（RSD=4.4%）, respectively, which indicated that the established method was accurate, stable and feasible. And the whole detection process was completed in about three minutes. The contents of 2 components in 4 batches of Homalomena occulta were 0.328-0.398 mg·g^-1（linalool）and 0.559-0.630 mg·g^-1 （protocatechuate）, respectively.

The ¹H-q NMR method has the advantages of simple operation, fast analysis speed and specificity, and can be used for the simultaneous determination of two active components in Homalomena occulta, providing a scientific basis for the overall quality evaluation and quality control of Homalomena occulta.

To determine the content of acrylamide in “8 famous medicines from Zhejiang”, and to carry out the preliminary risk assessment based on the determination results.

After optimization of QuEChERS extraction, the content of acrylamide was determined by the method of isotope-labeled internal standard-ultra high performance liquid chromatography-tandem mass spectrometry (isotope-labeled IS-UHPLC-MS/MS). The determination was carried out with a Phenomenex Kinetex C₁₈ column (100 mm×2.1 mm, 1.7 μm) as the stationary phase, gradient elution was carried out with methanol-0.1% formic acid aqueous solution as the mobile phase, ¹³C₃ acrylamide as the internal standard, and multiple reaction monitoring (MRM) mode was used to detect the residual acrylamide.

The content ranges of acrylamide in 247 batches of samples were 0-26 403 μg·kg^-1. These contents exceeded the regulations stipulated by some nations or organizations, and posed certain safety risks in long-term use.

The method established in this study is rapid, simple, sensitive and reproducible, and will lay a scientific basis for the quality control and safety evaluation of acrylamide in “8 famous medicines from Zhejiang” and other genuine medicinal materials.

To determine the in vitro release degree of musk sustained-release mini-tablets by reciprocating cylinder method.

Gas chromatography was used to establish the in vitro analysis of muscone, which is the main active ingredient of sustained-release mini-tablets. Comparing its equilibrium solubility in different concentrations of Tween-80, hexadecyl trimethyl ammonium bromide (CTAB) and sodium dodecyl sulfate (SDS), to determine the type of release medium. The effects of residence time, drip time, reciprocation rate, and screen mesh sizes on the release behaviours of muscone were investigated. Results were compared with that of the paddle method. Meanwhile, a preliminary investigation into the mechanism of its release was also carried out.

The linearity of the constructed analytical method was better, the RSD values of precision, repeatability and stability were less than 3%, and the spiked sample recovery was qualified. The release medium for the reciprocating cartridge method was 200 mL of 0.05% Tween-80, with a dwell and drip time of 20 s, a reciprocation rate of 15 dip·min^-1, and upper and lower screen mesh sizes of 20 and 40 respectively. Compared with the paddle method, Muscone was completely released under different pH conditions in the reciprocating cylinder method, and the release curve increased smoothly.

The study can provide some references for the reciprocating cylinder method in the in vitro evaluation of sustained-release prescriptions of traditional Chinese medicine.

To establish a method for determination of potential anti-vascular disease active components of Semen raphani based on cell membrane chromatographic (CMC) model of human umbilical vein cell (HUVEC).

The HUVEC cell membrane chromatography coupled with HPLC-ESI IT TOF MS system were used to screen the active components of Semen raphani. The selected active components were further applied to ox-LDL induced HUVEC to verify their protective effects.

Two retained components were selected from Semen raphani by this method. One component was identified as erucinic acid by comparing with the reference material. Compared with the model group, the cell survival rates of the erucinic acid pretreatment groups increased significantly. The amount of ICAM-1 and VCAM-1 decreased in a dose-dependent manner. Bcl-2 protein levels decreased and Bax protein levels increased, with statistical significance (P<0.05).

The method can rapidly obtain active ingredients from complex traditional Chinese medicines. It provides a reference for the application of cell membrane chromatography and the development of Semen raphani.

To establish an ultra-high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) for the simultaneous determination of daidzein, formononetin, genkwanin, quercetin, rutin, apigenin, kaempferol, luteolin and puerarin in Tongfu Jingyaotong tincture.

The Waters ACQUITY UPLC HSS T3 Column (100 mm×2.1 mm, 1.8 μm) was used with methanol and 0.1% formic acid (gradient elution) as the mobile phase at a flow rate of 0.3 mL·min^-1. Column temperature was 45 ℃, and injection volume was 2.0 μL. Electrospray ion source was adopted with positive and negative ion modes and multi-reaction monitoring and acquisition.

Apigenin, genkwanin and daidzein had good linearity in the range of 0.2-1 000 ng·mL^-1, puerarin, rutin, luteolin, kaempferol and formononetin in the range of 0.2-2 000 ng·mL^-1, and quercetin in the range of 1.0-5 000 ng·mL^-1. The resolution was good, and the RSDs of precision, repeatability, reproducibility and stability test were all below 5% (n=6). The average recoveries ranged from 82.7% to 111.8% with RSDs (n=6) of 2.0%-5.4%. The contents of daidzein, formononetin, genkwanin, quercetin, rutin, apigenin, kaempferol, luteolin and puerarin in 6 batches of Tongfu Jingyaotong tincture were 8.46-17.97 μg·mL^-1, 0.62-1.67 μg·mL^-1, 0.03-0.08 μg·mL^-1, 1.34-2.22 μg·mL^-1, 0.70-1.14 μg·mL^-1, 0.48-0.99 μg·mL^-1, 0.20-0.90 μg·mL^-1, 0.10-0.16 μg·mL^-1 and 167.95-227.75 μg·mL^-1, respectively.

This method has strong specificity, wide linear range, accuracy and efficiency, and can detect the contents of 9 active ingredients in Tongfu Jingyaotong tincture at the same time, which offers an effective quality control method for Tongfu Jingyaotong tincture.

To establish an HPLC characteristic chromatogram of Xifeng Huoluo capsules, and to determine the contents of gastrodin, amygdalin, strychnine, hydroxysafflower yellow A, brucine, paeoniflorin, ferulic acid, salvianolic acid B, cryptotanshinone, tanshinone Ⅰ, and tanshinone ⅡA.

Extraction of 75% methanol was analyzed by a Venusil MP C₁₈ chromatographic column (250 mm×4.6 mm, 5 μm) using 0.1% phosphoric acid (A) -acetonitrile (B) as the mobile phase with gradient elution at a flow rate of 1.0 mL·min^-1. The column temperature was 30 ℃. The detection wavelengths were variable. The characteristic chromatograms of 10 batches of Xifeng Huoluo capsules were evaluated by similarity evaluation, and the eleven identified index components were quantitatively determined.

There were thirty-one common peaks in the characteristic chromatograms of eleven batches of samples and the similarities were all above 0.99. The common peaks could ascribed to twelve medicinal materials, and eleven of them were identified. Eleven components showed good linearity within their respective ranges (r≥0.999 4), and the average recoveries were 99.3%-103.0% with RSDs of 1.5%-2.4%.

The established method has high sensitivity and strong specificity. The HPLC characteristic chromatogram combined with multi-component quantitative determination can fully reflect its inherent quality and can be used for the quality control of Xifeng Huoluo Capsules.

To compare the differences of the volatile oil components of Pimpinella thellungiana Wolff extracted with different methods by GC-MS combined with retention index.

Volatile oil of Pimpinella thellungiana Wolff were extracted using steam distillation, salting-out assisted steam distillation and enzymatic hydrolysis-assisted steam distillation. The chemical components of volatile oil extracted by different methods were analyzed by GC-MS combined with retention index, while the relative contents of volatile oil components were calculated by peak area normalization method.

Among the three extraction methods, the extraction rate of volatile oil was as follows, enzymatic hydrolysis-assisted steam distillation > salting-out assisted steam distillation ≈ steam distillation method. The most comprehensive types of volatile oil were extracted by salting-out assisted steam distillation, followed by enzymatic hydrolysis-assisted steam distillation, and finally by steam distillation. The main types of the volatile oil components of Pimpinella thellungiana Wolff extracted with different methods were basically unchanged, but the relative contents of various compounds were different. A total of 47 compounds were identified from the volatile oil extracted with the three methods, including 35 common compounds. The main chemical structural types of these compounds were terpenes, terpenes, terpenoids, aromatics and aliphatics, among which the higher content compounds were β-bisabolene（17.25%-19.42%）, caryophyllene oxide （12.90%-15.70%）, 1-(3-methyl-2-butenoxy)-4-(1-propenyl) benzene （5.02%-9.36%） and β-pinene （5.31%-6.62%）.

The chemical composition types and relative contents of the volatile oil of Pimpinella thellungiana Wolff extracted with different methods are different, but the differences are not significant. The results can provide reference for the selection of suitable extraction methods and further utilization of volatile oil from Pimpinella thellungiana Wolff.

To establish a fast, accurate and sensitive method by UPLC-DAD-Q-TOF-MS/MS for the detection of 20 kinds of illegally added chemicals such as azilsartan, nifedipin, lacidipine、nebivolo in anti-hypertensive health foods.

Waters HSS T3 C₁₈（100 mm×2.1 mm, 1.8 μm ） column was used with mobile phase of 0.01 mol·L^-1 ammonium acetate aqueous solution-methanol and gradient elution（0 min, 5% A; 0-8 min, 5% A→95% A; 8-11 min, 95% A; 11-11.2 min, 95% A→5% A; 11.2-12 min, 5%). The flow rate was 0.3 mL·min^-1. The injection volume was 1 μL. ESI⁺, ESI^- scan and MS/MS mode were applied. Qualitative and quantitative analyses were carried out by UPLC-DAD-Q-TOF-MS/MS.

The method was validated. A good linear relationship was showed in the concentration of 1-50 μg·mL^-1, （RSD<3%）and the recovery was obtained in range of 80.5%-98.7%. Illegally added chemical drugs were found in 15 batches of samples tested by this method. Two or more types of drugs were detected in 14 batches of samples. Torsemide, candesartan cilexetil, lacidipine were detected in 9 samples. Lacidipine and nebivolol were found in one of the sample.

This method is fast, accurate and sensitive with a high degree of separation. It can be used as a powerful tool for the fast detection of illegally added chemicals in anti-hypertensive health foods.

To establish a UPLC-MS/MS method for the simultaneous determination of 47 pesticide residues in Sucrose.

The residues in the sample were extracted by acidic acetonitrile, concentrated by blow dry with nitrogen gas and then analyzed by using LC-MS/MS with multiple reaction monitoring(MRM). Blank matrix standard curve with internal standard method was used to determine the residue contents.

Each substance to be tested had good linearity relationship within certain concentration (r>0.995). The limits of quantification (LOQ) were 0.01-2.00 μg·kg^-1. The recoveries of 47 pesticide residues at three levels of 10, 25 and 50 μg·kg^-1 were from 71.0% to 106.0% with the RSD of 0.90%-8.5% in sucrose. 2 batches in 15 batches of sucrose samples were detected thiamethoxam and thiamethoxam, while the rest were not detected.

The method is simple, rapid and characterized with acceptable sensitivity and accuracy to meet the requirements of the determination of analysis, and this developed procedure is suitable for the determination of pesticide residues in Sucrose, can be used for quality control of sucrose.

To establish and optimize a rapid direct analysis of real time tandem mass spectrometry (DART-MS/MS) method for the rapid detection of 12 benzodiazepines in blood and urine that can be used in forensic toxicology work.

A DART ion source was used in conjunction with an API4000 Q Trap mass spectrometer. A DART 12Dip-It^TM autosampling module with a module travel speed of 0.6 mm·s^-1, a sample volume of 5 μL, and a gate voltage of 200 V were applied. The mass spectrometry section scans in positive ion mode using multiple reaction monitoring (MRM) mode. After further optimization, the DART-MS/MS method was validated and applied to real case samples.

Ethyl acetate was selected as the extractant for liquid-liquid extraction and the temperature of the carrier gas heater was optimized. The method has good selectivity and does not interfere with delayed effects. The linearity was good, and the limits of detection (LODs) for the targets in blood and urine were in the ranges of 0.5-10 ng·mL^-1 and 0.2-2 ng·mL^-1, respectively. And the limits of quantification (LOQs) were in the ranges of 1-50 ng·mL^-1 and 0.5-5 ng·mL^-1, respectively. The recoveries ranged from 78.8% to 119%, and the matrix effects ranged from -17.5% to 18.5%. The intra- and inter-day precisions were not greater than 14.4% for the high and intermediate concentrations, and not greater than 18.1% at the limits of quantification. This method enables fast and accurate examination of case samples.

The method is fast and convenient, with good sensitivity, and can be applied to the research and work of rapid detection of toxicants to improve the efficiency of detection.