It’s been about 10 years since authorities found the industrial chemical melamine¹  in milk products that sickened many children in China. Since then, the country’s food industry has responded with national crackdowns to stop dangerous illegal additives from making their way into the nation, and into the global food market. Unfortunately, some problems persist.

In the last decade, we have witnessed an increase in wellness and healthy living awareness, which has driven demand for health products including herbal supplements and remedies. Because of fierce market competition, manufacturers try to demonstrate the best consumer results. The fraudulent adulteration of products has become an issue. It can involve modifying herbal health products by fortifying them with additives or drugs.² These unlabeled and unregulated additions are a significant public concern because of their impact on the safety and authenticity of widely available products.

Sibutramine and phenolphthalein, for instance, have been found in many weight loss products.^3,4 While these hidden ingredients can provide consumers with quick results, they may also induce serious adverse effects such as drug dependence, liver damage, and tachycardia.⁵ This is only one example of why it is crucial that official regulations be in place to control the content of herbal health foods.

In Singapore, therapeutic health products are regulated by the Health Sciences Authority (HSA) under the Health Products Act (HPA)⁶ and the Health Products (Therapeutic Products) Regulations 2016⁷.

The EU legal framework for human medicines sets standards to ensure a high level of public health protection and the quality, safety and efficacy of authorized medicines. The requirements and procedures for marketing authorization, as well as the rules for monitoring authorized products, are primarily described in Directive 2001/83/EC⁸ and Regulation (EC) No 726/2004⁹.

The China National Food Safety Supervision and Sampling Implementation Guidelines (2017 version)¹⁰ have established monitoring parameters for health products. This guide covers the monitoring of 68 drugs in 6 different categories of health products.

As investigations of such products are increasingly important for public safety, analytical methods to effectively detect permissible amounts as stipulated by local regulations are just as critical. There are several techniques used to analyze products for additives, such as DNA barcoding.  In 2015, New York authorities used this method to conduct tests on top-selling store herbal supplements.¹¹ This approach has received some criticism by industry advocacy groups for its tendency to produce false positives .^12-13

Mass spectrometry for authenticity or adulteration

Figure 1. Complex mass spectrometry with QTRAP System involves one sample injection for simultaneous quantification and qualification.

Food testing laboratories require high sensitivity and selectivity when testing herbs and botanicals. This is where liquid chromatography with tandem mass spectrometry (LC-MS/MS) can help to detect and potentially identify chemicals of particular masses in the presence of other substances.

Most common mass spectrometric techniques for food testing utilize multiple reaction monitoring (MRM) mode as the gold standard for sensitivity and selectivity. However, in complex matrices such as plant products, even this technique can produce matrix effects such as matrix suppression or interference by matrix isobaric species which muddle the detection of the target analytes. Possible consequences include retention time and ion ratio discrepancies which can cause false peaks and false positives that interfere with detection and quantification.

Figure 2. Screening workflow using QTRAP System enables full scan confirmation of drug identity with database search.

To overcome these challenges, SCIEX QTRAP® Systems use a uniquely integrated MRM-IDA-EPI scanning mode. This provides MRM spectral peaks and enhanced secondary fragments with just one sample injection. MRM ion channel chromatographic peak quantification and EPI generated secondary spectra form a “fingerprint” spectrum. QTRAP System technology’s enhanced product ion (EPI) functionality allows for the collection of complete MS/MS spectra to cross-reference with an integrated library, for confirmation of the identity of the detected peak.

The following method¹⁴ was developed on the QTRAP System to detect the 68 health products in the 2017 National Food Safety Supervision and Sampling Implementation Guidelines. It also includes a secondary library to help users search, identify, and enhance the efficiency of monitoring and analysis. This monitoring protocol includes these advantages:

1. Covering all drug types, this method includes all drug additives to health products that must be detected per the 2017 National Food Safety Supervision and Sampling Implementation Guidelines.
2. With one sample injection and simultaneous positive and negative mode scanning, it is quick and easy.
3. This method includes sample preparation, MRM ion pair data, instrumentation methods, and secondary search libraries. This comprehensive solution on the QTRAP System includes the advantage of simultaneous quantitative and qualitative validation with a single sample injection.
4. This comprehensive solution satisfies multiple user needs. In use, it improves work efficiency and saves time.
5. Secondary search databases have high, medium, low, and combined energy fragment spectra. They contain a large amount of fragment information and effectively exclude false positives.

The above introduction is primarily extracted from the SCIEX technical note RUO-MKT-02-6399-A. For more details of the content, please download the technical note from https://sciex.li/2b1u3e

¹ https://www.bbc.com/news/10565838

²https://www.hsa.gov.sg/docs/default-source/announcements-csg/hsa-updates/hsaupdates_foreign-alert-_2018_july_aug-250918.pdf

³https://www.hsa.gov.sg/docs/default-source/announcements/safety-alerts/foreign-alert_2019_sep_oct_final-19feb2020.pdf

⁴https://www.hsa.gov.sg/docs/default-source/default-document-library/hsapr-clinic-k_rozell_pr_final_website98440db77ad94b96b5fc8fb43af2719a.pdf

⁵https://www.webmd.com/heart-disease/atrial-fibrillation/medicines-raise-heart-rate

⁶https://sso.agc.gov.sg/Act/HPA2007

⁷https://sso.agc.gov.sg/SL/HPA2007-S329-2016

⁸https://eur-lex.europa.eu/legal-content/EN/TXT/PDF/?uri=CELEX:02001L0083-20121116&qid=1472567249742&from=EN

⁹https://eur-lex.europa.eu/LexUriServ/LexUriServ.do?uri=OJ:L:2004:136:0001:0033:en:PDF

¹⁰http://www.qjqfda.com/WS01/CL1605/169718.html

¹¹ https://well.blogs.nytimes.com/2015/02/03/new-york-attorney-general-targets-supplements-at-major-retailers/?_r=0

¹² http://cms.herbalgram.org/press/2015/ABCSaysNYAttyMisusedDNA.html?ts=1423253839&signature=57878efd484887ada61087d06017df57&ts=1424965317&signature=c647affbb8859cca6f0f96c6a8eae7fe

¹³ https://pdfs.semanticscholar.org/7a55/e107ba65cb52156473580f4c8b0da48a207b.pdf

¹⁴ https://sciex.li/2b1u3e

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