Quantitative Analysis of Pesticides in Dietary Supplement by GC/MS/MS



Accurate analysis of pesticide in dietary supplement sample becomes more and more important.  The compendium pesticide methods can’t cover all dietary supplements which have various and complex matrices. We must develop a fast, simple, specific, sensitive and comprehensive method to quantify 112 pesticides in botanical and nonbotanical dietary supplement.

Method Development

Method development consists of Sample Preparation, Sensitivity Issue, Peak Tailing Issue, and Matrix Effect Issue.

Sample Preparation – Extraction Solvent

We must adopt the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) technique.

We must also optimize the extraction solvent. Currently, the AOAC method solvent and USP method solvent do not do this. Only the Dyad method solvent has this capability.

Sample preparation – dSPE

Dispersive solid phase extraction (dSPE) is a simple, low cost, fast and sorbent-based technique to clean up a sample. Different dSPEs were compared, and Agilent 5982-5122 dSPE was selected.

Sample Preparation – Low Recovery

Some pesticides have low recovery since they stick to the surface of containers during extraction. The analyte protectant (AP) can prevent this low recovery issue by occupying the container surface.

Sensitivity Issue – dMrm and RTL

Too many Multiple Reaction Monitoring (MRM) transitions can cause low sensitivity issue. A dynamic MRM(dMRM) mode can keep sensitivity by setting up different time segments for many analytes. dMRM requires consistent retention times. Retention Time Locking (RTL) ensures the consistency of retention time by adjusting as flow rate.

Peak Tailing Issue – AP with Sandwich Injection Mode

Some pesticides have peak tailing issue, which is caused by stickiness to the GC system. AP with hydroxyl groups can block active sites in GC system to prevent peak tailing issue.

Matrix Effect – Internal Standard (IS) Selection

USP 561 uses only one IS. AOAC 2007.01 uses two IS. Dyad Labs uses five IS.

Matrix Effect – MRM Transition Selection

Each pesticide has three MRM transitions. Choose the transition with most sensitive and least interference to minimize matrix effect.

Method Validation

Method validation consists of: specificity, linearity and sensitivity, accuracy and range, precision, stability, and batch size.

Specificity: Method specificity is evaluated by analyzing blank diluent, blank matrix extract, analyte only and IS only. No significant contribution/interference peaks were observed in these samples.

Linearity and Sensitivity: Each pesticide has its own limit. Five different curve ranges were designed to cover all 112 pesticides using 9 standard curve points. The curve regression type is quadratic with weigh of 1/x and R2 must be 0.995.


This pesticide method is simple, fast, specific, sensitive and comprehensive. This pesticide method has been successfully validated in both botanical and non-botanical dietary supplement. This pesticide method has been successfully applied for proficiency test samples.