AQA (Analytical Qualit assurance ) responsibility?

AQC processes are of particular importance in laboratories analysing environmental samples where the concentration of chemical species present may be extremely low and close to the detection limit of the analytical method In well managed laboratories, AQC processes are built into the routine operations of the laboratory often by the random introduction of known standards into the sample stream or by the use of spiked samples

Quality control begins with sample collection and ends with the reporting of data ( S very important to be be noted dears AQC is achieved through laboratory control of analytical performance. Initial control of the complete system can be achieved through specification of laboratory ☄services,☄ instrumentation ☄glassware,☄ reagents,☄ solvents, and ☄gases. However, evaluation of daily performance must be documented to ensure continual production of valid data. A check should first be done to ensure that the data should be seen is precise and accurate.  Next, systematic daily checks such as analysing ☄blanks, ☄calibration ☄standards, quality control check ☄samples, and references must be performed to establish the reproducibility of the data. The checks help certify that the methodology is measuring what is in the sample.

The quality of individual AQC efforts can be variable depending on the training, professional pride, and mportance of a particular project to a particular analyst. The burden of an individual analyst originating AQC efforts can be lessened through the implementation of quality assurance programs. Through the implementation of established and routine quality assurance programs, two primary functions are fulfilled: the determination of quality, and the control of confidence ( S -Really) By monitoring the accuracy and precision of results, the quality assurance program should increase confidence in the reliability of the reported analytical results, thereby achieving adequate AQC (Analytical quality control)

[As per experience AQA ? its framework to monitor for Quality in Quality control complete activities its should have defined SOP in the work r activities responsibilities Quality control generation all documents under custody Quality control for A to Z training Quality control generated all results should be checked should be before (FP/API) QA Quality control for incidence/deviations/OOS/CAPA/CC/ call respective should go to QA via AQA (then that original QA) If any results in electronic signature same checked by in quality control person ( Review) after results should confirm AQA Organogram/JD for arranging all persons ( QA/QC) etc.,

AQA – also should have trend for all like OOS/OOT/Incidence/Deviations/APQR (FP/API/RM/PM/CALIBRATION/TI SHEETS RESULTS etc.,

AQA- Quality control What are using any type of documents should be authorized by AQA /AQC r QA

ANALYTICAL METHOD VALIDATION?

ANALYTICAL METHOD VALIDATION?

👉🏻DEFINATION:
Analytical Method Validation:
Validation of an analytical procedure is the process by which it is established, by laboratory studies, that
the performance characteristics of the procedure meet the requirements for the intended analytical
applications.
👉🏻🎯Specificity:
Ability to assess unequivocally the analyte in the presence of components which may be expected to be
present (impurities, degradants, matrix). It is a measure of the degree of interference from such things as
other active ingredients, excipients, impurities, and degradation products, ensuring that a peak response
is due to a single component only.
👉🏻🎯Precision:
The precision of an analytical procedure expresses the closeness of agreement (degree of scatter)
between a series of measurements obtained from multiple sampling of the same homogeneous sample
under the prescribed conditions. Precision may be considered at three levels: repeatability, ☄intermediate
precision and ☄reproducibility.
Repeatability (Method Precision):
Repeatability expresses the precision under the same operating conditions over a short interval of time.
Repeatability is also termed intra-assay precision.
👉🏻🎯Intermediate precision (Ruggedness):
Intermediate precision expresses within-laboratories variations: different days, different analysts,
different equipment, etc.
🎯🙋🏼‍♂🎯👉🏻Accuracy:
The accuracy of an analytical procedure expresses the closeness of agreement between the value which
is accepted either as a conventional true value or an accepted reference value and the value found.
🏃🏻‍♀🏃🏼🏃🏻‍♀🏃🏼🏃🏻‍♀🏃🏼Linearity:
The linearity of an analytical procedure is its ability (within a given range) to obtain test results which
are directly proportional to the concentration (amount) of analyte in the sample.
😎👴🏿👠💄💃🏼🙋🏼Range:
The range of an analytical procedure is the interval between the upper and lower concentration
(amounts) of analyte in the sample (including these concentrations) for which it has been demonstrated
that the analytical procedure has a suitable level of precision, accuracy and linearity.
👉🏻🎯Detection Limit (DL/r 📞LOD is Limit of Detection 🤔🎯☺):
The detection limit of an individual analytical procedure is the lowest amount of analyte in a sample
which can be detected but not necessarily quantitated as an exact value.👉🏻🎯Quantitation Limit (QL r 📞Limit of quantification ):
The quantitation limit of an individual analytical procedure is the lowest amount of analyte in a sample
which can be quantitatively determined with suitable precision and accuracy. The quantitation limit is a
parameter of quantitative assays for low levels of compounds in sample matrices, and is used
particularly for the determination of impurities and/or degradation products.
👉🏻🎯👴🏿Robustness:
The robustness of an analytical procedure is a measure of its capacity to remain unaffected by small, but
deliberate variations in method parameters and provides an indication of its reliability during normalusage💊💊💊🙏🏽💊💊💊

Ultra-performance liquid chromatography (UPLC)? is involves HPLC with very high pressures and columns having very small particle sizes

Ultra-performance liquid chromatography (UPLC)? is involves HPLC with very high pressures and columns having very small particle sizes (.👈🏻😅?)

👉�Principle(🤔?)
The efficiency of HPLC increased as particle sizes of the column packing decreased from 10 [micro] m in the 1970s to 3.5 Nun in the 1990s🤔 (then now 1.25?😅)👉� This is shown by lower values of HETP (height equivalent to a theoretical plate) for van Demeter plots of HETP (column efficiency) versus mobile phase flow rate in units of linear velocity ([mu], mm/s & this particle size range, and even down to 2.5 Nun particles used in shorter columns in the early 2000s, it was found that HETP decreases to a minimum value and then increases with increasing flow rate. However, with the 1.7 [micro] m particles used in UPLC, HETP is lowered compared to the larger particles and does not increase at higher flow rates👉�This allow faster separations to be carried out on shorter columns and/or with higher flow rates, leading to column increased resolution between specific peak pairs 💞and increased peak capacity, defined as the number of peaks that can be separated with specified resolution in a given time interval🙌�🙌�

👉�Theory Of UPLC?
The chromatogram that depicts the elution of a solute is a graph relating the concentration of the solute in the mobile phase leaving the column to elapsed time. 👉�However, at a constant flow rate, the chromatogram will also relate the solute concentration to the volume of mobile phase passed through the column is shown the elution of a single peak📉📈The expression, f(v), is the elution curve equation and this will be derived using the plate theory.

☄Once the nature of f(v) identified, then by differentiating f(v) and equating to zero, the position of the peak maximum can be determined and an expression for the retention volume (Vr) obtained☄The expression for (Vr) will disclose those factors that control solute retention 🏋🏾
UPLC is a new separation technique with increased speed, sensitivity and resolution👉�The performance of a column can be measured in terms of the height equivalent to the theoretical plates (HETP or H), which is calculated from the column length (L) and the column efficiency, or number of theoretical plates (N) 👉�N is calculated from an analyst’s retention time (tR) and the standard deviation of the peak (σ). ☄ H = L/N ———— (1)
☄N=(tR/σ)2 ——– (2)

👉�The van Deemter equation is the empirical formula that describes the relationship between linear flow velocity (μ) and column efficiency, where A, B, and C are constants related to the mechanistic components of dispersion ( for me 😇)

H = L/N = A + B/μ + Cμ—- (3) (VAN DEEMTER EQUATION)

👉�According to the van Deemter plot, column efficiency is inversely proportional to the particle size (dp) (Equation 4🙄), so by decreasing the particle size there is an increase in efficiency⌛ Since resolution is proportional to the square root of N (Equation 5), decreasing particle size increases resolution☄⌛Also, by using smaller particles, analysis time can be decreased without sacrificing resolution, because as particle size decreases, column length can also be reduced proportionally to keep column efficiency constant💧 By using the same HPLC mobile phase and flow rate (🗣O👁C) UPLC™ reduces peak width and produced taller peaks which increased 📈📉the S/N 1.8 to 8 fold, improving both sensitivity and resolution b/w 13-18 😋

N α 1/dp ————— (4) R = √N/4(α-1/α)(k/k+1) ————— (5)😲💤🙄

🎯Also according to the van Deemter plot, use of particles smaller than 2 μm produces no loss in column efficiency with increasing flow rates🎯However, by increasing flow rates to decrease analysis time, there is a corresponding increase in system pressure🎯As a result, a system capable of withstanding the proper pressures while still maintaining efficiency is required🎯 As well, a mechanically stable column is needed.
💊💊💊🙏�💊💊💊