Most ReadThe components of biological samples are complex, and the concentration range of target analytes varies significantly. Therefore, sample pretreatment is particularly important for subsequent analysis. With the continuous development of analytical techniques, the requirements for sample pretreatment are also increasing. Pretreatment technologies are evolving towards microscale, time-saving, high-efficiency, online, and environmentally friendly directions to meet the requirements of complex matrices and trace analysis. Online pretreatment technologies integrate sample pretreatment steps and subsequent detection processes directly into an automated system, which can reduce steps and errors, improve analysis efficiency and sensitivity, and achieve automatic, rapid, and efficient analysis of target compounds. This paper reviews the online pretreatment technologies for biological samples in China and abroad in the past 10 years, offering valuable insights to guide future research and innovation in the realm of biological sample pretreatment.
This article focuses on the key experimental operations in the study about the applicability of microbial limit testing methods for drugs，summarizing literature and experience from the preparation of test solution，design of methods for microbial counting and control bacteria inspection，operation of microbial recovery test，bacterial liquid concentration counting，and operational methods for controlling bacterial & fungal purity. Emphasis was placed on the preparation methods of water-soluble test samples with strong antibacterial effects，non-oil and fat test samples that were not easily soluble and dispersed，and the test solution for oil and fat test samples. Detailed introduction of the sequential experimental plan for methods of aerobic bacterial count，mold & yeast count，and control bacterial inspection were introduced. Four operational methods for adding bacteria about membrane filtration were explained，and the impact of different ways of adding bacteria on the results of the method was analyzed. Summarized three counting methods for bacterial & fungal concentrations. Detailed sharing of operational experience on controlling the purity of bacterial solution. Summarized the current status about research on the applicability of microbial limit testing methods of drugs. Four suggestions for the future development of research on the applicability of microbial limit testing methods for drugs have been proposed：（1） Unify the operation about bacteria adding method in membrane filtration，scientific and reasonable；（2）Strengthen supervision of pharmaceutical production enterprises and review of microbial limit testing methods for drugs；（3）Unify the microbial limit testing methods for the drugs of the national sampling plan，and gradually collect and bind into a book；（4）Strengthen the research on the applicability of microbial limit testing methods for excipients.
To develop a flow-through cell method for the dissolution test of omega-3-acid ethyl ester 90 soft capsules and compare the dissolution behaviors from different manufacturers.
The medium (surfactant and its concentration, pH, dosage of pepsin), flow rate and system mode (closed versus open) were investigated. The samples were collected at the specified time and determined by HPLC. The similarity of the dissolution curves between generic drugs and reference listed drug was evaluated by similarity factor (f2).
A closed-loop mode of flow-through cell apparatus was employed, with 0.01 mol·L-1 hydrochloric acid solution containing 4.0% Triton X-100 as the dissolution medium, and the flow rate was 2.0 mL·min-1. The dissolution curves of the samples that have passed consistency evaluation are similar to those of the reference and the samples produced by enterprise in the declaration stage are partly similar. The method has effective distinguish ability for product quality and different prescriptions.
The newly established method can be used for the quality control of omega-3-acid ethyl ester 90 soft capsules, and can provide references for further consistency evaluation and the dissolution method development of lipid-filled soft gelatin capsule (SGC).
The national drug sampling and inspection project is an important way of drug quality supervision in China which providing strong support for drug supervision and standard improvement. This article summarizes the national drug sampling and inspection project of Arnebiae Radix completed by Institute for Control of Chinese Traditional Medicine and Ethnic Medicine，National Institutes for Food and Drug Control in 2015 and 2022. The results illustrated that the qualification rate of Arnebiae Radix has increased from 43.9% in 2015 to 87.5%，and the qualification rate of Arnebiae Radix has significantly increased. The two nationwide inspections of Arnebiae Radix reflected the scarcity of Arnebiae Radix resources in Xinjiang and Inner Mongolia，resulting in a high market share of unqualified samples. The thin layer identification spots of the unqualified Arnebiae Radix sampled in 2015 were not consistent with the qualified samples. The thin layer identification of the unqualified samples sampled in 2022 was consistent with those of the qualified samples，but the depth of the spots were not consistent with those of the qualified samples，indicating that the current unqualified samples were adulterated samples，which posing greater challenges to the quality supervision of Arnebiae Radix. Through the exploratory research of twice National Drug Sampling and Inspection Project，it is preliminarily believed that it is of great significance to improve the standard test items of Arnebiae Radix，scientifically establish the limit value and strengthen the construction of the quality control system for the supervision.
Objective: To develop an inductively coupled plasma mass spectrometry(ICP-MS) method for the determination of Cd, Pb, As, Hg, Co, V, Ni and Se in the crude drug of lanthanum carbonate. Methods: Samples were diluted with 3% nitric acid and directly injected. The matrix effect was eliminated by standard addition method and matrix matching method. Lanthanum oxide was added into the standard solution as the matrix.Compare the linearity, repeatability, accuracy, quantification limit, detection limit and sample determination results of the two methods by methodological validation and sample determination. Results: The linear ranges of ICP-MS standard addition method and matrix matching method were 0-30 ng · mL-1, the correlation coefficients for all elemental impurities were good(r>0.998). Limits of detection were between 0.003 9-0.22 ng · mL-1 and 0.009 1-0.72 ng · mL-1. The RSD of repeatability(n=6) were between 1.5%-4.9% and 5.1%-6.9%. The recoveries were between 87.0%-98.3% and 83.4%-114.4%. The contents of 8 elemental impurities in the crude drug of lanthanum carbonate were basically same. Conclusion: The established two methods can effectively eliminate the matrix effect. They were both simple, rapid, sensitive, accurate and applicable for the elemental impurity control of lanthanum carbonate.
To establish an in vitro permeation method for crisaborole ointment and to provide a reference for the bioequivalence of crisaborole ointment.
The HPLC method was used to determine the permeability of crisaborole ointment, and the vertical Franz diffusion pool method was used to study the release characteristics of the ointment in vitro. The chromatographic column was Thermo BDS Hypersil-C18(150 mm×4.6 mm, 5 μm), with 0.1% phosphoric acid solution-acetonitrile (60：40) as the mobile phase, flow rate of 1.5 mL·min-1, column temperature of 30 ℃, detection wavelength of 254 nm, and injection volume of 10 μL.
The peak shape of crisaborole in the chromatogram of the test sample was good. There was no peak at the position of crisaborole in the negative sample chromatogram, which did not interfere with the determination. The linear relationship of crisaborole was good within the range of 0.026-21.02 μg·mL-1 (r≥0.999). In six repeated experiments, the mean maximum transmittance (Jmax) of the self-made product and the reference formulation were compared (odds ratio: 0.94). Simultaneously calculate the confidence interval for Jmax, with a 90% confidence interval ranging from 87.9% to 102.0%. The mass conservation percentage of each sample was 94.1%-101.1%(n=12). The reference solution was left at room temperature for 26 h, with a peak area RSD of 0.44%. The self-made product and reference preparation were left in a water bath at room temperature and 32 ℃ for 26 h, with peak area RSD ranging from 0.78% to 1.1%, indicating good stability of the solution. For the three batches of samples tested, the ratio of the mean Jmax values of the self-made product and the reference formulation was within the range of 0.92-0.97. Simultaneously calculate the confidence interval for Jmax, with a 90% confidence interval ranging from 84.8%-100.7%.
This method is simple and convenient to operate, with high selectivity, strong exclusivity and high accuracy.
In the process of drug development，the bioanalytical is required generally in pharmacokinetic studies. The accuracy，reliability，and scientificity of bioanalytical method validation are crucial，the investigation of matrix effects has become an important part of the validation system for bioanalytical methods. This article investigated related guidelines from ICH，NMPA，FDA and EMA，searching the related domestic and foreign literature on matrix effect，combining with the case study of matrix effect in actual review，to discuss the method of investigating the matrix effect in the methodological verification of drug concentration detection in unknown biological samples，to clarify the causes and solutions of matrix effect. So as to ensure the standardization of the methodological verification of drug concentration detection in unknown biological samples and the accuracy of the test results，to achieve the optimization of drug concentration detection methods for biological samples.
Objective: To establish a two reference substances for determination of multiple components (TRSDMC)method for the simultaneous determination of scutellarin, rosmarinic acid, negletein, carvacrol and thymol in Moslae Herba, which was more economical and effective for the quality control of Moslae Herba. Methods: The retention times of the five components in Moslae Herba were determined using HPLC on 13 different C18 columns. The average retention time of each component under each column was then used as the standard retention time for that component.Rosmarinic acid (peak 2) and carvacrol (peak 4) were chosen as linear calibration standards. The chromatographic peaks were localized by using liner calibration with two reference substances (LCTRS). Rosmarinic acid was used as the control substance to determine the content of each component using a relative correction factor. And the results were compared with those obtained from the external standard method. Chemometric analysis was used to excavate the differential quality markers of Moslae Herba. Results: LCTRS had accurate prediction results for the measured components and enjoyed a wide range of column applications. The correction factors of scutellarin, negletein, carvacrol and thymol to rosmarinic acid were 0.853 3, 0.475 2, 3.034 7 and 2.738 6, respectively, and their relative standard deviations were below 2.0%.There was no significant difference between contents obtained by the two methods. The contents of scutellarin, rosmarinic acid, negletein, carvacrol and thymol in 21 batches of Moslae Herba were 0.05-2.87 mg · g-1, 0.73-9.73 mg · g-1, 0.04-0.99 mg · g-1, 0.36-8.52 mg · g-1 and 0.61-10.2 7 mg · g-1, respectively. The 24 batches of samples could be clustered into three categories, and thymol, carvacrol and negletein ether could be used as differential quality markers. Conclusion: TSDMC method for the simultaneous determination of the contents of 5 components in Moslae Herba is stable and reliable, and provides a new idea for the overall quality control of Moslae Herba.
Objective: To identify and analyze the chemical components of Bufei Jianpi formula by ultra-high performance liquid chromatography-coupled with high-resolution mass spectrometry (UPLC-HRMS). Methods: A Hypersil GOLD (2.1 mm×100 mm, 2.6 μm) column was used. Methanol (A)-0.1% formic acid water (B) was used as the mobile phase with gradient elution, the flow rate was 0.2 mL · min-1, and the column temperature was 30 ℃.The mass spectrometry data were collected using the Full MS/dd-MS2 scanning mode of positive and negative ions, and the characteristic fragment ion peak information was analyzed by compound discoverer. Combined with Chemspider, mzCloud and other databases and existing reports of relevant chemical composition information,the chemical components of Bufei Jianpi formula was analyzed by using the cracking prediction of Mass Frontier and its cracking rule. Results: A total of 221 compounds were identified from Bufei Jianpi formula, including 65 flavonoids, 40 phenylpropanoids, 21 terpenoids, 16 alkaloids and 79 other compounds. Conclusion: UPLC-Orbitrap Fusion Lumos Tribrid-MS can quickly identify the chemical components of Bufei Jianpi formula and qualitatively analyze the material basis of Bufei Jianpi formula, which can be used for the quality control of Bufei Jianpi formula.
Althought mRNA vaccines have been developed for nearly 30 years，but due to certain technical bottlenecks in production，stability，and reactivity，the development of mRNA vaccines has been relatively slow. During the epidemic of COVID-19，mRNA vaccine had been fully verified its effectiveness and safety for preventing infectious diseases. Here，this article summarized the key quality control attributes and related requirements of mRNA vaccine products for preventing infectious diseases by reviewing the quality control guidance documents of WHO and drug regulatory and standardization agencies，aiming to provide reference for the quality control of mRNA vaccine products for preventing infectious diseases in China.
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